CN1083920C

CN1083920C - tissue paper containing a fine particulate filler

Info

Publication number: CN1083920C
Application number: CN96194514A
Authority: CN
Inventors: 肯尼思·D·文森; 约翰·P·埃斯帕默; 查尔斯·W·尼尔; 杰夫里斯·P·霍尔特
Original assignee: Paper Science & Technology Inst
Current assignee: Paper Science & Technology Inst
Priority date: 1995-04-07
Filing date: 1996-03-27
Publication date: 2002-05-01
Anticipated expiration: 2016-03-27
Also published as: EP0819195A1; ATE210225T1; PT819195E; KR19980703689A; CZ323697A3; AU721197B2; ZA962500B; NZ305665A; DK0819195T3; EP0819195B1; ES2169236T3; CA2217520A1; KR100264040B1; DE69617662D1; AU5373196A; CN1187226A; DE69617662T2; BR9610752A; WO1996031653A1; HUP9800978A2

Abstract

Strong, soft, and low dusting tissue paper webs useful in the manufacture of soft, absorbent sanitary products such as bath tissue, facial tissue, and absorbent towels are disclosed. The tissue papers comprise fibers such as wood pulp and a non-cellulosic, water insoluble particulate filler such as kaolin clay.

Description

The tissue paper that contains fine particulate filler

Technical field

Put it briefly, the present invention relates to creped tissue paper product and method.More precisely, the present invention relates to creped tissue paper product by the preparation of the water insoluble microparticle filler of cellulose pulp and non-cellulose.

Background of invention

The toilet paper tissue paper product has obtained extensive use.These products are supplied in market with all size and are used for various uses such as face tissue, toilet paper and absorbefacient towel paper.The specification of these products promptly quantitatively, thickness, intensity, page size, batching (dispensing medium) etc. have very big-difference usually, but their contact is common production method, promptly so-called crepe paper manufacture method.

Wrinkling is the method that mechanically compresses page in paper machine direction.The result makes quantitatively (weight per unit area) to increase, and great variety has taken place many physical properties, particularly in the physical property of paper machine direction detection.Wrinklingly normally use pliable and tough blade, the relative Flying Dutchman of a kind of so-called scraper is finished in the mode of operation on the machine.

Flying Dutchman is normally large diameter, the roller of 8-20 foot (244-610 centimetre), and it is designed to the used vapour pressurization, to produce the surface of heat, finishes the drying of paper web when purpose is the paper-making process end.Paper web as forming on the fourdrinier wire, does not need a large amount of water to come loosen collagen fibre suspension at first at porose shaping carrier here; Then, the shaping paper web is transferred on the woollen blanket or fabric of so-called press section, and the dehydration here is continuous, or by the dehydration of mechanical compaction page, or by some other dewatering such as hot blast impingement drying; At last, page is transferred to the Flying Dutchman surface to finish drying with leather hard.

Various creped tissue paper products again by the consumer to the contact of the joint demand of one group of physical property of common contradiction together, these physical properties are: comfortable sense of touch, i.e. pliability, and have high strength simultaneously and resist to fall hair and anti-dry linting.

Pliability is by the consumer who holds specific paper product, wrinkles the sense of touch of being felt through skin friction and with hand.This sense of touch is the combination of several physical properties.Those of ordinary skill in the art it has been generally acknowledged that one of most important physical property relevant with pliability is to make the deflection of the paper web of this product, and deflection is considered to directly depend on the intensity of paper web usually.

Intensity is that this product and its constitute paper web keep physical integrity under service condition, and anti tear, the ability of breaking and tearing up.

Fall hair and dry linting be meant that paper web is handled or discharge between the operating period not in conjunction with or in conjunction with the not firm fiber or the tendency of particulate filler.

Creped tissue paper normally is made up of paper fibre basically.Usually comprise also that a spot of chemical functional auxiliary agent as wet strong or do strong adhesive, keep auxiliary agent, surfactant, sizing agent, chemical softening composition, be convenient to wrinkling composition, but the consumption of these auxiliary agents is very little usually.The paper fibre that is most commonly used to creped tissue paper is former chemical wood pulp.

Because the economy that the natural resources supply in the world is subjected to increasing day by day and the influence of Environmental Studies, the pressure that reduces the consumption of the former chemical wood pulp in forest product such as the hygiene paper product will increase.Expanding given wood pulp supply and don't causing an impaired method of product quality is to replace former chemical pulp fiber with high yield fiber such as machinery or change machine slurry or with recycled fiber.Unfortunately, serious relatively performance destruction usually is accompanied by this variation.This fiber is easy to have high roughness, and this can make the VELVET impression of being given by selected fibrillation decrease, and this swan velvet is because fibrillation has flexibility.With regard to wandering fibre machinery or chemical machinery, high roughness is that this composition comprises lignin and so-called hemicellulose because the original timber material maintains the non-cellulose composition.This can make the weight of every fiber increase, and length is constant.Reclaim paper and also often contain very high content of mechanical pulp, still, even when carrying out as far as possible carefully that waste paper is selected so that content of mechanical pulp is reduced to when minimum, high roughness still often takes place.This is considered to, and mixture that paper by separate sources is mixed and made into abiogenous impure fibre morphology when reclaiming paper pulp causes.For example, because certain waste paper in fact mainly is the North America leaf wood, so it is selected; Yet people often find a large amount of dirts from more coarse needle-leaved wood fibre, or even from the most harmful seeds such as various U.S. south pine.The United States Patent (USP) 4,300,981 that on November 17th, 1981 was signed and issued to Carstens has illustrated the outward appearance quality and the surface quality of being given page by fibrillation, and this patent is incorporated into own forces in this for reference.Be signed and issued to the United States Patent (USP) 5 of Vinson on July 20th, 1993,228,954 and be signed and issued to the United States Patent (USP) 5 of Vinson April 11 nineteen ninety-five, 405,499 incorporate into own forces in this for referencely, and they disclose improves this fibre resources method for quality, so that their harmful effect reduces, but the replacement amount still is restricted, and the supply of this new fibre resources itself also is limited, and this has often limited their use.

The applicant has been found that another method that reduces wood pulp use amount in the toilet paper is to replace the part wood pulp with low cost, the filler that is easy to buy such as kaolin or calcium carbonate.Though the those of ordinary skill in this field will be recognized, this practice is thought very common in some part of paper industry always, but they also will realize, it is that much special difficulty is arranged that this method is applied to hygiene paper product, and this makes that this method does not obtain implementing up to now yet.

A kind of main restriction is the keeping of filler in the paper-making process.In paper product, toilet paper quantitatively minimum.When tissue webs when Yankee paper machine is rolled onto on the reel, it quantitatively generally only is about 15 gram/rice ², and because therefore wrinkle or the shortening that creping doctor produces, in fact hang down 10-20% than the dried fiber basis weight of finished product page in the dried fiber basis weight of the shaping of paper machine, squeezing and drying section.In order to solve the difficulty of keeping that quantitatively causes by hanging down, tissue webs has extremely low tightness, and the apparent tightness that twists on the reel only is about 0.1 gram per centimeter usually ³Or it is lower.Though people will appreciate that, at the creping doctor place, can quote some loft, but this field those of ordinary skill will recognize, tissue webs is normally formed by the slurry of free relatively shape, this show the fiber of forming page be not because of making beating limpen.By practice, thin-paper machine need be in very high-speed operation down; Therefore, free beaten stock need be avoided too much forming pressure and drying load.The stiff relatively fiber that comprises free beaten stock is in the ability that pine is dredged state when keeping them to make initial sheet forming.The those of ordinary skill in this field can recognize at once that during sheet forming, this low quantitative, low tightness structure will can not infiltrated fine particles effectively.The filler grain that is not fixedly attached to fiber surface can be taken away by the torrent of high speed flow apperach, pours liquid phase, and enters from the water that the shaping paper web leaches by initial paper web.Have only to repeat to reclaim to be used to be shaped the water of paper web, the concentration of particulate just can reach a point, and this moment, filler began to leave away with page.This solid concentration in the waste water is unpractical.

Second kind of major limitation is that the particulate filler mode that paper fibre tends to interosculate when can not be with the shaping paper web dry is attached on the paper fibre naturally.This has reduced the intensity of product.The filler inclusions can cause that intensity reduces, if it can not get suitably keeping in paper, and can the quite use of weak product of serious restriction.Recovering the needed step of intensity also often is restricted as the fiber making beating of increase or the application of chemical intensifier.

Filler also often causes the adverse effect of page integrality and stops up the squeezing blanket or can not be well transfer to Flying Dutchman and the pollution problem that produces from press section.

At last, the tissue paper product that contains filler is easy to hair or dry linting.This is not only because filler itself can not kept in paper well, and because they have above-mentioned combination and are suppressed effect, this part that can cause the fiber that anchors at this structure weakens.This tendency can make in the processing operation of crepe paper manufacture process and postorder and produce operating difficulties, because the too much dust that page produces when handling.What another will be considered is, requires this product not fall hair and dry linting relatively by the user who adds the hygiene paper product that the tissue paper filled out makes.

Therefore, the use in the paper made on Yankee paper machine of filler is severely limited always.The United States Patent (USP) 2,216,143 that was signed and issued to Thiele on October 1st, 1940 is incorporated into own forces in this for reference, and this patent has been discussed and use the suffered limiting factor of filler on Yankee paper machine, and discloses the integrated approach that overcomes those limiting factors.Unfortunately, the unit operations that this method need bother promptly when the blanket face of page contacts with Flying Dutchman, is coated with the bonding particle of one deck on this face.For modernized high speed Yankee paper machine, this operation is unpractiaca, and the those of ordinary skill in this field will be recognized that the Thiele method will produce coating rather than adds the tissue paper product of filling out." add the tissue paper of filling out " and be different from " coating tissue paper " and be its production method in fact, (filled tissue paper) is that fiber forms before the paper web promptly " to add the tissue paper of filling out ", particle matter is added in the fiber and the page of making, and " coating tissue paper " after to be paper web form basically, adds particle matter and the page made.Because this difference, add and fill out tissue paper product and can be called the relative low weight of on Yankee paper machine, making, the creped tissue paper of low tightness, this tissue paper contains and runs through the filler that is distributed at least one layer multi-layer tissue paper thickness or the whole thickness of individual layer tissue paper.Term " runs through dispersion " and is meant that all parts add the certain layer of filling out tissue paper product basically all contains filler grain, and still, this does not illustrate that this dispersion in this layer must be uniform.In fact, add thickness different in the packing course at tissue paper and obtain packing density difference, can reckon with some advantage.

Therefore, the purpose of this invention is to provide the tissue paper that contains fine particulate filler, this tissue paper has overcome the limiting factor of above-mentioned prior art.Tissue paper of the present invention is soft, and it contains the filler of keeping, and has high tensile strength and low dry linting value.

This purpose and other purpose can obtain with the present invention, as what instructed in following the disclosing.

Summary of the present invention

The present invention is that tissue paper is filled out in high strength, soft adding, and have hang down the hair and dry linting, it comprises the particulate filler of paper fibre and non-cellulose, and the weight that said filler accounts for said tissue paper is at least about 5% to nearly 50%, but is more preferably 8-20%.Fill creped tissue paper by particulate filler with this tittle, obtained unexpected pliability, intensity and anti-dry linting in conjunction with effect.

In preferred embodiments, of the present invention adding, fill out tissue paper and have about 10-50 gram/rice ²Quantitatively, more preferably 10-30 gram/rice ²Its tightness is about 0.03-0.6 gram/rice ³, and 0.05-0.2 gram/rice more preferably from about ³

Embodiment preferred also comprises the paper fibre of leaf wood and needlebush kind, is leaf wood at least about 50% paper fibre wherein, and is needlebush at least about 10%.Leaf wood and needle-leaved wood fibre most preferably divide and open into different layers, and wherein this tissue paper comprises internal layer and at least one skin.

Preferred tissue paper of the present invention is the pattern densification, and therefore, high relatively tightness district is distributed in the high bulk zone, comprises the tissue paper of pattern densification, and high relatively tightness district wherein is continuous, and the high bulk district is discontinuous.Most preferably, this tissue paper is the hot blast impingement drying.

The invention provides the creped tissue paper that comprises paper fibre and particulate filler.In its preferred embodiment, particulate filler is selected from clay, calcium carbonate, titanium dioxide, talcum, alumina silicate, calcium silicates, hibbsite, active carbon, pearl starch (pearl starch), calcium sulfate, glass microballoon, diatomite and composition thereof.When from top one group of material, selecting filler, need the appraisal Several Factors.These comprise cost, validity, be easy to be retained in the tissue paper, color, scattering energy, refractive index and with the chemical compatibility of selected papermaking environment.

Have now found that a kind of particularly suitable filler is a kaolin.With compare most preferably so-called " alumina silicate of hydration " type kaolin by the kaolin of calcining further processing.

Kaolinic form is natural flat or block, but preferred use is not subjected to the clay that mechanical delamination is handled, because mechanical delamination meeting reduces average particle size.In general, be meant average particle size with regard to suitable sphere diameter.In the invention process, preferred average suitable sphere diameter is greater than about 0.2 micron, more preferably greater than about 0.5 micron.Most preferably, suitable sphere diameter is greater than about 1.0 microns.

Unless stated otherwise, all percentages, ratio and ratio here all is by weight.

Brief description of the drawings

Fig. 1 is the schematic diagram of the crepe paper manufacture method of the present invention of explanation production high strength, softness and the creped tissue paper that hangs down hair, and this tissue paper comprises paper fibre and particulate filler.

Fig. 2 is illustrated as the schematic diagram of making creped tissue paper and preparing the step of moisture papermaking batching, and it is based on one embodiment of the invention of cationic flocculant.

Fig. 3 is illustrated as the schematic diagram of making creped tissue paper and preparing the step of moisture papermaking batching, and it is based on another embodiment of the invention of Flokal B.

Detailed description of the present invention

Although this explanation can believe that to particularly point out and to explicitly call for the end that is considered to content of the present invention the present invention can be understood preferably from the reading of following detailed description and appended examples.

Just as used herein, term " comprises " and refers to can be used in combination various compositions, component or step when enforcement is of the present invention.Therefore, term " comprise " comprise more restrictive term " basically by ... form " and " by ... composition ".

Just as used herein, term " water-soluble " refers at 25 ℃ to have the material of 3% dissolving (by weight) at least in water.

Just as used herein, term " tissue webs, paper web, (paper) width of cloth, page and paper product " all refers to the page by the method manufacturing that comprises the following step; These steps comprise: form moisture papermaking batching, batching is deposited on the porose surface, as fourdrinier wire, and by the drainage of gravity or vacuum aided, squeeze under the situation that has or does not have, and get rid of water by evaporation from prepare burden.Last step is included in leather hard page is adhered to the surface of Flying Dutchman, by evaporating into draining, makes page reach the substantially dry state, by pliable and tough creping doctor, removes paper web from Flying Dutchman then, and final page is rolled onto on the reel.

Just as used herein, term " adds the tissue paper of filling out " and refers to the paper product that can be called relative low weight, low tightness creped tissue paper, it is made on Yankee paper machine, comprises the filler that runs through the whole thickness that is distributed at least one layer multi-layer tissue paper thickness or individual layer tissue paper.Term " runs through dispersion " and refers to add basically the certain layer of filling out all parts of tissue paper product and all contains filler grain, and still, this does not illustrate that this dispersion in this layer must be uniform.In fact, obtain packing density difference, can reckon with some advantage at the packing course different-thickness that adds of tissue paper.

The commutative in the prior art use of term " the multi-layered tissue paper width of cloth, multi-layer web, multilayer (paper) width of cloth, multiple ply dheet and multi-ply paper product ", they refer to by page two-layer or that the moisture papermaking batching of multilayer is made, these layers are preferably by dissimilar fibrous, as used in the tissue paper manufacturing, these fibers are generally long relatively needlebush and relative short broad-leaved wood fiber.These layers preferably form on the one or more endless band hole pattern surface by independent dilution fibrous suspension is deposited into.If on the porose net surface that separates, form each layer at the beginning, subsequently with each layer combination (during hygrometric state) with the formation multi-layered tissue paper width of cloth.

Just as used herein, term " monolithic tissue paper product " refer to the paper product formed by a slice creped tissue paper, this sheet come down to homogeneous or it can be the tissue webs of multilayer.Just as used herein, term " multi-ply tissue paper product " refers to that it is made up of the above creped tissue paper of a slice.Each sheet in the multi-ply tissue paper product come down to homogeneous or they can be the tissue webs of multilayer.

The first step of the inventive method is to form at least a " moisture papermaking batching ", and just as used herein, this term refers to the suspension of paper fibre, normally is made up of wood pulp and particulate filler and additive.These additives are for providing particulate filler to keep effect and being necessary by selectively comprising any other function that the modified chemical product that describe below obtain.Some typical components in the papermaking batching are described in following part.

The component of papermaking batching

Paper fibre

May expect that the wood pulp of all kinds will be contained in the paper fibre of the present invention usually.Yet, other cellulose fibre slurry, as cotton linter, bagasse (bagasse), synthetic paper dimension (rayon) etc. also can be used, and is not all abandoned.Wood pulp used among the present invention comprises chemical pulp, for example sulfite pulp and sulfate pulp (being also referred to as kraft pulp sometimes) and mechanical pulp for example comprise ground wood pulp, thermomechanical pulp (TMP) and CTMP (Chemi-Thermomechanical pulp) (CTMP).The paper pulp that is obtained by deciduous tree and coniferous tree also can use.

Can adopt the paper fibre of the blend of hardwood pulp and softwood pulp and two kinds of slurries as tissue paper of the present invention.Term " hardwood pulp " refers to the fiber pulp that obtains from the xyloid material of deciduous tree (angiosperm) as used herein; And " softwood pulp " is the fiber pulp that the xyloid material from coniferous tree (gymnosperm) obtains.The broad-leaved wood sulphate pulp particularly mixture of eucalyptus and northern needlebush sulfate (NSK) slurry is made tissue paper of the present invention with being particularly suitable for.A preferred embodiment of the present invention comprises the tissue webs of stratification, and wherein, most preferably, hardwood pulp such as eucalyptus slurry are used for skin, and wherein, northern softwood kraft pulp is used for internal layer.The low-cost paper dimension that is obtained by reclaimed waste paper also can be used for the present invention, and reclaimed waste paper can comprise the fiber of any kind of or all mentioned kinds.

Particulate filler

The invention provides the creped tissue paper that comprises paper fibre and particulate filler.In its preferred embodiment, particulate filler is selected from clay, calcium carbonate, titanium dioxide, talcum, alumina silicate, calcium silicates, hibbsite, active carbon, pearl starch, calcium sulfate, glass microballoon, diatomite and composition thereof.When from top one group of material, selecting filler, need the appraisal Several Factors.These comprise cost, validity, be retained in easiness in the tissue paper, color, scattering energy, refractive index and with the chemical compatibility of selected papermaking environment.

Have now found that a kind of particularly suitable particulate filler is a kaolin.Kaolin is a kind of common name of spontaneous physalite material, and it is selected with particulate form.

About term, be noted that in industry and prior art patent documentation, when relating to kaolin product or adding man-hour, refer to not kaolin through calcining with term " hydration ".Calcining makes kaolin be subjected to high temperature more than 450 ℃, this temperature change kaolinic basic crystal structure.So-called " hydration " kaolin can be produced by selected natural kaolin, for example, and froth flotation, magnetic separation, mechanical layering, pulverizing or similarly grind, but the heating of the damage crystal structure of not mentioning to some extent.

On the accurate technique meaning, it is inappropriate that these materials are called hydration.More precisely, in kaolin structure, in fact there is not molecular water.Therefore, though its composition can and often the people for being write as 2H ₂OAl ₂O ₃2SiO ₂Form, but people think that always kaolin is that proximate composition is Al ₂(OH) ₄Si ₂O ₅Silicic acid aluminium hydroxide, it is equal to the hydration chemical formula of just having mentioned.In case kaolin is subjected to calcining [concerning the purpose of this specification, being that the high temperature of instigating kaolin to be subjected to more than 450 ℃ is handled to eliminate hydroxyl through time enough], so original kaolin crystal structure will be damaged.Therefore, though say technically, this burnt clay no longer is " kaolin ", but in paper industry, people generally call these kaolin of calcining, and, concerning this specification, when mentioning " kaolin " class material, in calcined materials is also included within.Therefore, term " aluminium hydrosilicate " is a natural kaolin, and it does not pass through calcination processing.

When enforcement was of the present invention, aluminium hydrosilicate was most preferred kaolin form.Therefore, its feature is, is about 13% (weight) at high temperature more than 450 ℃ with the above-mentioned loss of water vapour form.

Kaolinic form is natural flat or bulk, because it is with the natural generation of sheet form, thin slice adheres to again and forms " lamination " or " piece " shape together, adds man-hour, and this laminated kaolin is separated to a certain degree just becomes single thin slice.But the preferred clay of handling without too much mechanical delamination that uses is because mechanical delamination tendency is in reducing average particle size.In general, average particle size is with regard to suitable sphere diameter.In the invention process, preferred average quite sphere diameter is greater than about 0.2 micron.More preferably greater than about 0.5 micron.Most preferably, suitable sphere diameter is greater than about 1.0 microns.

The clay of most exploitations will be subjected to wet processing.The aqueous suspension of natural clay makes coarse impurity to remove by centrifugal, and provides medium for chemical bleaching.Sometimes in this suspension, add polyacrylate polymers or phosphate to reduce viscosity and to slow down sedimentation.Final clay generally loads and transports under the not drying of about 70% solid suspension, or can spray drying.

Processing to clay, as air flotation, froth flotation, washing, bleaching, spray drying, interpolation is as the auxiliary agent of suspension stabiliser and viscosity modifier, acceptable normally, and should select based on concrete economic situation present in the specific environment.

Every kind of multi-silicate aluminium that clay platelet itself all is a sandwich construction.Continuously arranged oxygen atom forms the one side of each basic unit.Polysilicate chip architecture edge is coupled together by these oxygen atoms.The continuously arranged hydroxyl of the octahedra aluminium oxide structure that links together has formed other face that constitutes two-dimentional polymerization oxidation constructed of aluminium.The oxygen atom of sharing tetrahedron and octahedral structure has been attached to the aluminium atom on the silicon atom.

The defective of this structure mainly is to make the natural clay particle have anionic charge in suspension.This takes place because other two, three and quadrivalent cation replace aluminium.The result makes more lip-deep oxygen atoms become anion, and becomes weak dissociable hydroxyl.

Natural clay also has cationic characteristic, and it can convert anion to preferred other ion.This situation be because produce the aluminium atom that lacks abundant complementary key sometimes at the surrounding edge of thin slice.They must satisfy their remaining chemical valences by attract anion from the aqueous suspension that is occupied.If these cation-bits are not content with the anion from solution, clay can satisfy the charge balance of self to the surface of " card room " combining structure of forming thick dispersion by making own edge surface so.Polyacrylate dispersant carries out ion-exchange with the CATION point that clay is repelled, and just can avoid these combining structures and be simplified in the use of production, shipment and clay.

A kind of WW FiL SD ^The kaolin of board is spray-dired kaolin, is to be sold by the Dry Branch kaolin company of Georgia State DryBrauch, is suitable for making the creped tissue paper width of cloth of the present invention.

Starch

Of the present invention aspect some, be useful as one of component of papermaking batching with starch.When particulate filler and fiber exist, in water, have limited deliquescent starch of the present invention particularly useful aspect some, this will describe in detail in the back.The common means that obtains this effect is to use so-called " cationic starch ".

Just as used herein, term " cationic starch " can be described as starch, and it is natural acquisition, and by chemical modification to give the cationic substituent part.Preferred this starch obtains from corn or potato, also can obtain as rice, wheat or cassava from other source.Particularly preferably be the starch from waxy maize of the industrial amioca of being called starch.Amioca starch is different from common dentation cornstarch, and it is amylopectin all over, and common cornstarch contains amylopectin and amylose.The characteristic of the various uniquenesses of amioca starch also is described in " Amioca-The Starch form waxyCorn " [H.H.Schopmeyer, Food Industries, in December, 1945; The 106-108 page or leaf] in.This starch can be granular or dispersed granular, pre-gelatinization.Preferably dispergated.If pre-gelatinization is granular, only need be dispersed in before use in the cold water, to notice that simultaneously use equipment overcomes the tendency that produces blob of viscose when forming dispersion liquid.The suitable disperser that is called injector is used always in this industry.If starch is granular and not pre-gelatinization, need cooking starch so that the particle swelling.Preferably, as by boiling this state before the dispersion that starch granules is swelling to just will become starch granules.The starch granules of this height swelling is referred to as " well-done fully ".The condition of dispersion liquid changes with the size of starch granules, the degree of crystallinity of particle and the content of amylose usually.For example by the heating of the water slurry of the starch granules of 4% concentration being made complete well-done amioca starch in about 30-40 minute at about 190 °F (about 88 ℃).

Cationic starch generally can be divided into following a few class: (1) uncle's aminoalkyl ether, and (2) kind of starch ether comprises quaternary amine, p and s derivative, the starch powder of (3) primary and secondary aminoalkyl starch and (4) other kind (as, imino group starch).New CATION product is also continuing exploitation, and still, uncle's aminoalkyl ether and quaternary ammonium alkyl ether are main industrial products.Preferably, cationic starch has the substitution value of the about 0.01-0.1 cationic substituent of every grape sugar acid anhydride unit's starch; Preferably from the substituting group of type above-mentioned.The starch that is fit to is with RediBOND by national starch and chemical company (Bridgewater, New Jersey) ^Trade mark is produced.The starch that has cationic moiety has only as RediBOND 5320 ^With RediBOND 5327 ^Be fit to, have the starch such as the RediBOND 2005 of additional anionic functional degree ^Also be suitable for.

Although be not wishing to be bound by theory, it is believed that initial water-soluble cationic starch can become insoluble when filler exists, this is because of its sucking action to anion point on the filling surface.This can make filler be covered by a large amount of starch molecules, and this starch molecule attracts the surface for more filler grain provides, and finally causes the agglomeration of filler.The key factor that it is believed that this step is the size and the shape of starch molecule, rather than the charge characteristic of starch.For example, with the linear polymerization electrolyte replacement cationic starch of material as synthesizing of electric charge deflection, obtained the effect of difference.

In one embodiment of the invention, preferably cationic starch is added in the particulate filler.In this case, based on the weight of carbon granules filler, the cationic starch amount of interpolation is about 0.1-2%, but 0.25-0.75% most preferably.In this one side of the present invention, preferably use cationic flocculant as keeping auxiliary agent.

In another embodiment of the invention, preferably cationic starch is added in the whole moisture papermaking batching to a preferred position before the mixing pump dilution in the end.This respect of the present invention utilizes Flokal B as keeping auxiliary agent.In this respect of the present invention, preferably the ratio that coagulates agent with about 5-20 times anion etc. adds cationic starch.

CATION above-mentioned and Flokal B will be in following detailed descriptions.

Keep auxiliary agent

Many materials are sold as so-called " keeping auxiliary agent ", term just as used herein, and it is meant in paper-making process, is used for increasing the fine furnish solids thing and keeps additive at paper web.The tiny solid thing can not get enough keeping, they or can be lost in the technique waste water or in the whitewater closure loop of circulation, gather too high concentration, thereby cause and produce difficulty, comprise sediment pile and reduce the efficient of drainage.The 17th chapter (slurry and the paper that are entitled as " keeping chemistry ", chemistry and chemical technology, the third edition, the 3rd volume, J.E.Unbehend and K.W.Britt, A Wiley Interscience Publication) type and the mechanism that promoter effect is kept in polymerization has been carried out necessary explanation, and it incorporates into own forces in this for reference.Flocculant makes the particle agglomeration of suspension usually by bridge formation mechanism.Though some polyvalent cation is considered to common flocculant, in practice, they are replaced by the significant polymer of effect usually, and this polymer has many electric charge points along polymer chain.

Cationic flocculant

Can use " cationic flocculant " effectively to produce according to tissue paper product of the present invention as keeping auxiliary agent.Just as used herein, this term refers to a kind of polyeletrolyte.These polymer are normally produced by one or more olefinic unsaturation monomer copolymerizations, and monomer wherein is generally acrylic monomers, forms or comprise cationic monomer by cationic monomer.

The cationic monomer that is fit to be dialkyl aminoalkyl-(methyl) acrylates or-(methyl) acrylamide, or with hydrochlorate or with the form of quaternary ammonium salt.The alkyl that is fit to comprises dialkyl amido ethyl (methyl) acrylates, dialkyl amido ethyl (methyl) acrylamide and dialkyl amino ylmethyl (methyl) acrylamide and dialkyl amido-1,3-propyl group (methyl) acrylamide.These cationic monomers preferably with non-ionic monomer, preferred acrylamide copolymerization.Other polymer that is fit to is polymine, polyamide epichlorohydrin polymer and as the diallyldimethylammonium chloride monomer, the homopolymers and the copolymer of common and acrylamide.

Be suitable on paper, all can be used for making according to product of the present invention as any common CATION synthesized polymer flocculant of keeping auxiliary agent.

Compare with the chondritic of cationic starch, the preferred line style of this polymer.

Though preferred intermediate density, the charge density of wide range is useful.The polymer that is used to make product of the present invention comprises the Cationic functional groups that frequency is 0.2-2.5 milliequivalent/gram polymer, but more preferably 1-1.5 milliequivalent/gram polymer.

Be used to make polymer according to tissue paper product of the present invention and should have molecular weight at least about 500,000, preferred about molecular weight more than 1,000,000, the most preferably molecular weight more than 5,000,000.

The example of acceptable material is RETEN 1232 ^With Microform 2321 ^, the cation polyacrylamide emulsion of polymerization and the RETEN 157 that transmits with solid particulate form ^These all are the products of the Hercules company in Delaware, USA Wilmington city.Another acceptable cationic flocculant is Accurac 91, a kind of product of the Cytec company in Stamford city, CT state.

This field those of ordinary skill will recognize that the desirable consumption of these polymer will alter a great deal.Based on the dry weight of this polymer and the dry weight of finished product tissue paper, be low to moderate about 0.005% amount of polymers (by weight) and also can produce useful effect, but in general, the consumption of requirement is higher; With regard to the present invention, when using these materials, even can be higher than general actual amount.May use high extremely about 0.5% amount, but in general, amount the best of about 0.1%.

Flokal B

In another aspect of this invention, " Flokal B " is a kind of useful components.Here employed " Flokal B " refers to have the heavy polymer of CATION side group.

Anionic polymer often has carboxylic acid (COOH) part.These parts can tightly hang (pendant) to main polymer chain or generally by alkylidene (alkalene) group, particularly have the alkalene group of several carbon to be hanging to main chain.In water-bearing media (except when hanging down the pH value), this hydroxy-acid group ionization is to give the polymer negative electrical charge.

The anionic polymer that is suitable for Flokal B is not that the monomeric unit that is easy to produce hydroxy-acid group during all or basically by polymerization is formed, but by not only producing nonionic but also producing that the combination of monomers of anionic degree of functionality forms.Produce the monomer of non-ionic functionalities, if particularly have polarity, it shows the tendency of flocculation that homo-ion degree of functionality is identical through regular meeting so.Owing to this reason, in actual the use, often mix this monomer.Often the non-ionic monomer that uses is (methyl) acrylamide.

Anionic polyacrylamide with relative high molecular is suitable flocculant.This anionic polyacrylamide comprises (methyl) acrylamide and (methyl) acrylic acid combination, mix when wherein the latter can be by polymerization that acrylic monomers obtains or the hydrolysis by some (methyl) acrylamide monomer after the polymerization obtains, or obtain by the method that combines.

Compare with the chondritic of anionic starch, this polymer preferably is line style basically.

Very wide charge density is useful, though preferred intermediate density.It is 0.2-7 milliequivalent/gram polymer or higher Cationic functional groups that the polymer that is used to make product of the present invention comprises frequency, but more preferably 2-4 milliequivalent/gram polymer.

An example of acceptable material is RETEN 235 ^, it is a solid particulate form, is a kind of product of the Hercules company in Wilmingyton city, the Delaware State.Another acceptable Flokal B is Accurac 62 ^, be a kind of product of the Cytee company in Stamford city, CT state.

This field those of ordinary skill will recognize that the consumption of these polymer will alter a great deal.Based on the dry weight of finished product tissue paper, be low to moderate about 0.005% amount of polymers (by weight) and also can produce useful effect, but in general, the consumption of requirement is higher; With regard to the present invention, when using these materials, even can be higher than general actual amount.May use high extremely about 0.5% amount, but in general, amount the best of about 0.1%.

Other additive

Other material also can be added to moisture papermaking batching or initial paper web with give product other characteristic or improve papermaking process, as long as the chemical of these materials and selected particulate filler is compatible, and the influence that can not produce significant adverse to pliability of the present invention, intensity or low dry linting characteristic.Following material is clearly included, but is not comprehensive.Other material also can be included, as long as they can not influence or reduce benefit of the present invention.

The material of cationic charge deflection is added to paper technology to control the Zeta potential of moisture papermaking batching when it is transported to paper technology, and this is very common.Why use these materials to be because the most solid thing has negative electrical charge with regard to surface in nature, comprise the surface of cellulose fiber peacekeeping particulate and most of inorganic fillers.Many experts in this field think, the material of cationic charge deflection is desirable, and these solids because it has partly neutralized make them be easier to that cationic starch and cationic polyelectrolyte flocculate as previously mentioned by cationic flocculant.The deflection cationic charge additive of Shi Yonging is an alum traditionally.Recently, in this field, use low-molecular-weight relatively cation synthesising copolymer to carry out electric charge deflection and handle, the molecular weight of this polymer preferably is not more than about 500,000 and more preferably no more than about 200,000 or even about 100,000.The charge density of this low molecular weight cationic synthetic polymer is higher relatively.These charge density are about 4-8 equivalent cationic nitrogen/kg of polymer.A kind of suitable material is Cypro 514 ^, a kind of product of the Cytec company in Stamford city, CT state.In practical range of the present invention, clearly allow to use this material, but be careful in use.Yet, as everyone knows, though this reagent in a small amount just can by neutralization be not easy near the anionic centers of bigger flocculation molecule and so the repulsion that reduces particle help keep, yet, because these materials can be fought for anion fixation point (anchoring site) with cationic flocculant, thus, when the anion point has in limited time, opposite owing to the actual effect that the negative interaction of keeping is made they and expectation.

In order to improve shaping, drainage, intensity and to keep, this area that is applied in of high surface, high anionic charge particulate has obtained good understanding.See the United States Patent (USP) 5,221,435 that for example was signed and issued to Smith on June 22nd, 1993, it incorporates into own forces in this for reference.The common material that is used for this purpose is a colloid, silica or bentonite.Adding these materials clearly comprises within the scope of the invention.

If expectation obtains permanent wet strength, can add following chemicals to papermaking batching or initial paper web so: polyamide-epichlorohydrin resins, polyacrylamide, styrene-butadiene latex; Insoluble polyvinyl alcohol; Ureaformaldehyde; Polymine; Chitosan polymer and its mixture.The polyamide epichlorohydrin resin is the CATION wet strengthening resin, and it has been found has special effectiveness.This resin that is fit to type is described in the following patent: the United States Patent (USP) that was signed and issued to keim on October 24th, 1972 was signed and issued to the United States Patent (USP) 3,772,076 of Keim on November 13rd, 3,700,623 and 1973, and it incorporates into own forces in this for reference.A kind of commercial source of useful polyamide-epichlorohydrin resins is the Hercules company in Wilmington city, the Delaware State, and the said firm is with Kymene 557H ^Trade mark is sold this resin.

Many crepe paper products all must have limited wet strength, because they need enter putrefaction or sewerage is disposed by the lavatory.If these products have wet strength, temporary wet strength so preferably, its feature is that when water existed, its some or all wet strength effects descended.If expectation obtains temporary wet strength, can select the resin of dialdehyde starch or other band aldehyde degree of functionality so for use, as the Co-Bond 1000 that sells by national starch and chemical company ^, by the Parez 750 of Stamford city, CT state Cytec company sale ^With the resin that is described in the United States Patent (USP) 4,981,557 that was signed and issued to Bjorkquist on January 1st, 1991, this patent is incorporated into own forces in this for reference.

Strengthen absorbability if desired, can use surfactant to handle the creped tissue paper width of cloth of the present invention.Based on the dry fiber weight of tissue paper, the amount of used surfactant preferably is about 0.01-2.0%.Surfactant preferably has the alkyl chain of 8 or more carbon atoms.Typical anion surfactant is the alkylsulfonate and the alkylbenzenesulfonate of line style.Typical non-ionic surface active agent is an alkyl glycoside, comprises that alkyl polyglycoside esters is [as Crodesta SL-40 ^, can buy from Croda company (New York, New York)]; Alkyl glycoside ether [being described in the United States Patent (USP) 4,011,389 that was signed and issued to W.K.Langdon etc. on March 8th, 1977]; [, can buy and IGEPAL RC-520 with the ester of alkyl polyethoxylated from Glyco chemical company (CT state, Greenwich city) as Pegosperse 200 ML ^, can buy from Rhone Poulenc company (New Jersey, Cranbury city)].

Chemical softening composition as selectable component particularly including interior.Acceptable chemical softening composition comprises well-known dialkyl dimethyl ammonium salt as two tallow dimethyl ammonium chlorides, two tallow dimethyl sulfate ammonium methyls, two (hydrogenation) tallow dimethyl ammonium chloride; Preferred two (hydrogenation) tallow dimethyl sulfate ammonium methyl.This special material can be bought from the Witco chemical company in Ohio Dublin city, and commodity are called Varisoft 137 ^Also can use one and two-ester variant of biodegradable quaternary ammonium compound, and at this

In the scope of invention.

The present invention also can use together with adhesive and the coating that design can spray on paper surface or the Flying Dutchman, and this product design is used to control the adhesion of paper web to Flying Dutchman.For example, incorporate into own forces to disclose and use the aqueous dispersion of polyvinyl alcohol to improve the method for paper web the adhesion of Flying Dutchman with certain degree of hydrolysis and viscosity in this United States Patent (USP) for reference 3,926,716 (Bates).This polyvinyl alcohol is with trade name Airvol ^Sold by Air product and chemical company (PA state, Allentown city), it can use with the present invention.Same recommend to be directly used on the Flying Dutchman or lip-deep other Flying Dutchman coating of page is cationic polyamide or polyamino resin, as by the Houghton international corporation in PA state Valley Forge city with trade name Rezosol ^And Vnisoft ^With by Delaware State Wilmington city Hercules company with trade name Crepetrol ^Those resins of making.These resins also can use with the present invention.Preferably, the adhesive by the polyvinyl alcohol resin that is selected from partial hydrolysis, polyamide, polyamino resin, mineral oil and composition thereof is fixed on paper web on the Flying Dutchman.More preferably be selected from the adhesive of polyamide epichlorohydrin resin, mineral oil and its mixture.

With regard to selectable chemical addition agent listed above, they only are exemplary, are not to be used for limiting the scope of the invention.

Moisture papermaking preparation of batch

Those of ordinary skill in the art will recognize, concerning the crepe paper manufacture method, not only the qualitative chemical composition of papermaking batching is important, and the relative quantity of each component and interpolation order and time and other factor also are very important.Have now found that following technology is suitable for preparing moisture papermaking batching, but should not think that the description of this technology defines scope of the present invention, the scope of the invention is limited by this explanation ending place appending claims.

Paper fibre is at first isolated single fiber by arbitrary common pulping process described in the prior and is prepared to form aqueous suspension.If necessary, then to the selected part of papermaking batching pull an oar (refining).Have been found that if will be used for the aqueous suspension of adsorbent particles filler subsequently pulls an oar and equal about 600ml Canadian Standard Freeness at least, but more preferably 550ml or below the 550ml, it is useful to keeping so.Dilution is favourable with the absorption of keeping auxiliary agent to polymer usually; Therefore, the suspension at this place or the solid content (by weight) that paper fibre suspension preferably is not higher than about 3-5% during preparation.

Selected particulate filler at first also is dispensed into aqueous suspension with it and prepares.Dilution is usually to polymer with to keep the absorption of auxiliary agent on the surface of solids favourable; Therefore, the suspension of the suspension at this place or particulate filler preferably is not more than the solid content (by weight) of about 1-5% during preparation.

One aspect of the present invention is based on cationic flocculant and keeps chemical action.It at first comprises interpolation starch, and when particulate filler existed, this starch had limited water-soluble.Preferably, this starch is cationic, and adds with the form of aqueous dispersion, and by weight, based on the dry weight of starch and particulate filler, the amount of starch is the aqueous suspension that 0.3-1.0% accurately joins the dilution of particulate filler.

Although when being not wishing to be bound by theory, it is believed that starch plays the agglomerant effect on filler, and cause the particle agglomeration.The agglomeration filler can make it more effectively be adsorbed onto the surface of paper fibre by this way.The absorption of filler on fiber surface can be passed through agglomerate suspension is mixed with at least a paper fibre suspension, and adds cationic flocculant and finish in final mixture.And although when being not wishing to be bound by theory, by building bridge between anion point on the paper fibre and the CATION point on the filler agglomerates, the flocculant effect at this place is considered to effective.

Cationic flocculant can add get the raw materials ready any suitable place in the approach flow of system of paper-making process to.Particularly preferably in adding cationic flocculant behind the mixing pump, at this, the circulation paper machine white water that is returned by technology has carried out last dilution to slurry.Shear section and can break the bridge that is formed by flocculant, therefore, common way is, moisture papermaking suspension add flocculant after many shearings that may run into section, this is well-known in field of papermaking.

A second aspect of the present invention is based on Flokal B.In this respect, preferably, this Flokal B adds the aqueous suspension of particulate filler at least to, and it separates with remaining aqueous papermaking batching basically simultaneously.Then, the mixture of Flokal B and particulate filler mixes with the part paper fibre at least, and cationic starch is added in the mixture; This mixing and interpolation starch were preferably finished before the last dilution of process, and here, the circulation paper machine white water is to be transported to head box with moisture papermaking batch mixes and by mixing pump.

Preferably, behind the interpolation starch, add the flocculant of additional dose again.Although in this one side of the present invention, the flocculant of initial dose is that anionic is necessary, the flocculant part of adding behind the mixing pump can be or anionic or cationic.Most preferably, the flocculant of second dosage adds be mixing pump after the last dilution with the circulation paper machine white water after.Shear section and can destroy a flocculate that is formed by flocculant, therefore, common way is, interpolation flocculants after many shearing that moisture papermaking suspension institute may run into section, and this is well-known in field of papermaking.

Those of ordinary skill in the art will recognize, shear section step minimum for making, and it is an exception that above-mentioned suggestion is directly added flocculant to particulate filler; Therefore, when anionic part flocculant at least added particulate to and adds particulate filler that material (it does not have other component of moisture papermaking batching basically) and flocculant handle in the end the section of dilution is added paper fibre to before, this respect of the present invention had produced unexpected benefit.The suitable ratio of Flokal B interpolation place is about 4: 1, and promptly for adding a total flocculation dosage behind the mixing pump, directly adding 4 parts is favourable in particulate filler.This rate of change is very big, and estimating to be fit to ratio can be from about 0.5: 1 to 10: 1, and this depends on the environment of variation.

When the product of either side of the present invention is represented in preparation,,, can use one or more suspension adsorbent particles fillers so according to the present invention if prepare multiple paper fibre suspension.Both made in paper technology, one or more paper fibre aqueous suspensions keep no particulate filler relatively before arriving mixing pump, also preferred CATION or the Flokal B of adding behind the mixing pump of this suspension.This is because the circulation plain boiled water that is used in the mixing pump place comprises filler agglomerates, and these filler agglomerates are failing to keep when hole sizer is arranged before this.When in the crepe paper manufacture process, using the fibrous suspension of multiple dilution, the liquid of CATION or Flokal B stream preferably adds the fibrous suspension of all dilutions to, and adds by this way: the liquid stream that makes flocculant matches with efflux of solids in the moisture papermaking batching of the fibrous suspension of each dilution.

In preferred scheme, preparation contains the short relatively paper fibre suspension of hardwood pulp, and is used to adsorb fine particulate filler, prepares the suspension of the long relatively paper fibre that contains softwood pulp simultaneously and makes it be in essentially no fine particulate filler state.Resulting staple fibre suspension directly flows to the mistress of three layers of head box, and forming the superficial layer of three layers of tissue paper, long fiber internal layer wherein flows out from the inner room of head box and forms, and long relatively paper fibre suspension has directly flowed to the inner room of head box.Final adding, fill out tissue webs and be particularly suitable for being processed into the monolithic tissue paper product.

In another preferred version, preparation contains the short relatively paper fibre suspension of hardwood pulp and is used to adsorb fine particulate filler, prepares the suspension of the long relatively paper fibre that contains softwood pulp simultaneously and makes it be in essentially no fine particulate filler state.The staple fibre suspension that obtains flows directly to a chamber of two chambers head box, to form one deck of double-deck tissue paper, wherein another long fiber floor is that second Room from head box flow out to form, and the suspension of long relatively paper fibre has directly flowed to second Room of head box.Final adding, fill out tissue webs and be particularly suitable for being processed into the multi-ply tissue paper product that contains biplate, and each sheet wherein all locate, so that make the surface of being made up of short relatively paper fibre that layer is positioned at the biplate tissue paper product.

Those of ordinary skill in the art also will appreciate that, directly flows to contiguous chamber by the moisture papermaking batching that makes same type, can reduce the apparent number of chambers of head box.For example, above-mentioned three Room head boxs also can be used as two Room head boxs, and this can be simply realizes by any that makes basically that identical moisture papermaking batching directly flows in two adjacent chamber.

With reference to Fig. 2 and Fig. 3, can further understand moisture papermaking preparation of batch method.Fig. 2 is illustrated as the schematic diagram that crepe paper manufacturing process prepares moisture papermaking batching, and this operation has produced according to the present invention the product of aspect, and this aspect is based on cationic flocculant.Fig. 3 is illustrated as the schematic diagram that crepe paper manufacturing process prepares moisture papermaking batching, and this operation has produced product according to a further aspect of the invention, and this aspect is based on Flokal B.Following discussion is with reference to Fig. 2:

Storage tank 1 is used to store the aqueous suspension of long relatively paper fibre.This suspension is carried by pump 2, and selectively by the strength potential of beater 3 with the long paper fibre of comprehensive raising.Charge pipe 4 is carried resin, to provide finished paper desired wet or dry strength.Then, this suspension is further adjusted in blender 5 to help the absorption of resin.Then, in mixing pump 6, dilute the suspension of adjusting through suitably, thereby formed the long paper fibre suspension 15 of dilution with plain boiled water 7.Pipe 20 has been added to suspension 15 with cationic flocculant, thereby has produced the long fiber suspension 22 of flocculation.

Still with reference to Fig. 2, storage tank 8 is containers storing fine particulate filler suspension.Charge pipe 9 is used to carry the aqueous dispersion of cationic starch additive.The effect of pump 10 is the dispersions of carrying fine particulate filler suspension and starch being provided.This suspension is to adjust in blender 12 to help the absorption of additive.Gained suspension 13 is transported to its place of mixing with the aqueous dispersion of staple fibre paper fibre through making beating.

Still with reference to Fig. 2, short paper fibre suspension comes from storage tank 11, and from storage tank 11, this suspension is transported to beater 15 through managing 49 by pump 14, and it has become the suspension 16 through the short paper fibre of making beating at this.With after the suspension 13 of fine particulate filler through adjusting mixes, it becomes the moisture papermaking suspension 17 of staple fibre base.Plain boiled water 7 mixes with suspension 17 in mixing pump 18, and at this, this suspension becomes the moisture papermaking suspension 19 of dilution.Pipe 21 directly adds cationic flocculant suspension 19, and after this, this suspension becomes the moisture papermaking suspension 23 of flocculation.

Preferably, the moisture papermaking suspension 23 of staple fibre base of flocculation is flowed directly in the crepe paper manufacture process illustrated in fig. 1, and be divided into two materials flows about equally, make it flow into head box chamber 82 and 83 then, develop into respectively at last adding of high strength, softness, low dry linting fill out creped tissue paper away from the layer 75 of drying cylinder one side and the layer 71 of drying cylinder one side.Similarly, with reference to Fig. 2, long paper fibre suspension 22 preferred streams of moisture flocculation are gone into head box chamber 82b, the intermediate layer 73 of filling out creped tissue paper that adds of developing into high strength, softness at last, hanging down dry linting.

Following discussion is with reference to Fig. 3:

Storage tank 24 is used to store the aqueous suspension of long relatively paper fibre.This suspension carry by pump 25 and selectively by beater 26 with the strength potential of the long paper fibre of comprehensive raising.Charge pipe 27 is carried resin, to provide finished paper desired wet or dry strength.Then, this suspension is further adjusted in blender 28 to help the absorption of resin.Then, in mixing pump 30, dilute the suspension of adjusting through suitably, thereby formed the long paper fibre suspension 31 of dilution with plain boiled water 29.Selectively, pipe 32 carries flocculant to mix with suspension 31, thereby forms the long fiber papermaking suspension 33 of moisture flocculation.

Still with reference to Fig. 3, storage tank 34 is containers storing fine particulate filler suspension.Charge pipe 35 is used to carry the aqueous dispersion of Flokal B.The effect of pump 36 is the dispersions of carrying fine particulate filler suspension and flocculant being provided.This suspension is adjusted in blender 37 to help the absorption of additive.Final suspension 38 is transported to the place of mixing with the aqueous dispersion of short paper fibre.

Still with reference to Fig. 3, short paper fibre suspension comes from storage tank 39, and from storage tank 39, this suspension is transported to the place that it mixes with fine particulate filler suspension 38 through adjustment through managing 48 by pump 40, to become the moisture papermaking suspension 41 of staple fibre base.Pipe 46 is carried the aqueous dispersion of the cationic starch that mixes with suspension 41 by on-line mixing device 50, thereby forms the suspension 47 of flocculation.Plain boiled water 29 flows directly into the suspension of flocculation, and they mix at mixing pump 42 places, becomes the moisture papermaking suspension 43 of staple fibre base of the flocculation of dilution.Selectively, pipe 44 is carried the flocculant of adding, and with the flocculation value of raising diluted suspension 43, thereby has formed suspension 45.

Preferably, short paper fibre suspension 45 from Fig. 3 is flow in the preferred paper-making process illustrated in fig. 1, and be divided into two approximately equalised materials flows, make it flow directly into head box chamber 82 and 83 then, become respectively at last adding of high strength, softness, low dry linting fill out creped tissue paper away from the layer 75 of drying cylinder one side and the layer 71 of drying cylinder one side.Similarly, with reference to Fig. 3, long paper fibre suspension 33 preferably flows directly into head box chamber 82b, the intermediate layer 73 of filling out creped tissue paper that adds that becomes high strength, softness at last, hangs down dry linting.

The crepe paper manufacture method

Fig. 1 is the schematic diagram that adds the crepe paper manufacture method of filling out creped tissue paper that explanation is used for production high strength, softness, low dry linting.These embodiment preferred are described in the following discussion, with reference to Fig. 1.

Fig. 1 is a side view of making the preferred paper machine 80 of page of the present invention.With reference to Fig. 1, paper machine 80 comprises the head box 81 (this head box 81 has a upper chamber 82, middle chamber 82b and end chamber 83) of a layering, pulpboard (slice roof) 84 and fourdrinier wire 85.Fourdrinier wire is formed a loop around breast roll (breast roll) 86, deflector (deflector) 90, suction flat box 91, couch roll (couch roll) 92 and several slewing rollers (turningroll) 94.In operation, a kind of papermaking batching is by upper chamber 82, second kind of papermaking batching is by middle chamber 82b, and the third batching forms initial paper web 88 (comprising 88a, 88b and 88c) by pumping in the end chamber 83 and concern outflow pulpboard 84 with position up and down, flowing on the fourdrinier wire 85.On fourdrinier wire, dewater, and by deflector 90 and suction flat box 91.When fourdrinier wire when direction of arrow operation is returned, before it begins to pass through breast roll 86 once more, it is cleaned by sparge pipe 95.At paper web transport zone 93, initial preparation 88 is owing to the effect of vacuum transfer suction box 97 is transferred on the porous carrier fabric 96.Support fabric 96 shifts from transition range 93 paper web through vaccum dewatering box 98, by blowing through predrying device (blow-through predryer) 100, and through two slewing rollers 101, the effect by pressure roller (pressure roll) 102 is transferred on the Flying Dutchman 108 then.When support fabric 96 through other slewing rollers 101, sparge pipe 103 and vaccum dewatering box 105, when finishing a circle, it is cleaned and dewaters.Be adhered to the cylindrical surface of Flying Dutchman 108 by adhesive by sprayer 109 coatings through the paper web of predry.On steam-heated Flying Dutchman 108 and by hot-air, finish drying.Hot-air is by not shown method heating and circulation in drying hood 110.Paper web is done wrinklingly from Flying Dutchman by scraper 111 then, and wrinkling back paper web is called page 70 (paper sheet), and page 70 comprises the layer 71, intermediate layer 73 of drying cylinder one side and away from the layer 75 of drying cylinder one side.Page 70 passes through between the felt wrapped rolls 112 and 113 and the circumferential section of spool 15, then coiled volume 116 on the fuse 117 of axle 118.

Still with reference to figure 1, the drying cylinder side layer 71 of page 70 is that the batching that the end chamber 83 by head box 81 pumps forms, and this batching directly is coated on the fourdrinier wire 85, and on fourdrinier wire, it has become the 88c layer of initial paper web 88.The intermediate layer 73 of page 70 is to be formed by the batching that the middle chamber 82.5 with head box 81 flows out, and this batching forms the 88b layer on the 88c layer.Page 70 is to be formed by the batching that the top chamber 82 from head box 81 flows out away from the layer 75 of a side of drying cylinder, and this batching forms the 88a layer on the 88b layer of initial paper web 88.Though Fig. 1 represents the paper machine 80 with head box 81 and can be suitable for preparing three layers paper web that yet adjustable whole head box 81 does not have layer, two-layer or other multi-layer web with preparation.

In addition, comprise page 70 of the present invention about preparation on the paper machine 80 of Fig. 1, fourdrinier wire 85 must have thinner sieve aperture, and these sieve apertures have less radius so that be shaped better with respect to the average length of the fiber of staple fibre batching.Porous carrier fabric 96 should have thinner sieve aperture, and these sieve apertures have less aperture with respect to the average length of the fiber of long fiber batching and go into space between the filament of fabric 96 with fabric one side of avoiding initial paper web basically.It is about 80% to be about the process conditions of preparation page 70 that paper web preferably is dried to before wrinkling, more preferably 95% fibre concentration.

Usually, the present invention can be used for creped tissue paper, and they comprise (but not and be confined to), the creped tissue paper of conventional woollen blanket squeezing; The creped tissue paper of high loosing character pattern densification, and high bulky, uncompacted creped tissue paper.

Of the present invention adding, fill out the creped tissue paper width of cloth and have 10-100 gram/rice ²Quantitatively.In its embodiment preferred, of the present invention adding, fill out tissue paper and have about 10-50 gram/rice ²Quantitatively, and 10-30 gram/rice most preferably ²Be suitable for the creped tissue paper width of cloth of the present invention and have about 0.60 gram per centimeter ³Or lower tightness.In its embodiment preferred, of the present invention adding, fill out tissue paper and have about 0.03-0.6 gram per centimeter ³Tightness, and 0.05-0.2 gram per centimeter most preferably from about ³

The present invention also can be used for the multi-layered tissue paper width of cloth.The tissue paper structures that is formed by the paper web of stratification is described in US3,994, (people such as Morgan Jr. in 771, on November 30th, 1976 issued), US4300981 (Carstens) issued on November 17th, 1981), US4166001 (people such as Dunning, on August 28th, 1979 issued) and European Patent Publication No 0613979A1 (people such as Edwards, on September 7th, 1994 is open), all patents are hereby incorporated by.Each layer is preferably by different types of fibrous.This fiber generally is long relatively needle-leaved wood fibre and relative short broad-leaved wood fiber, and is used in making as multi-layered tissue paper.Be suitable for the layer that the multi-layered tissue paper width of cloth of the present invention comprises two stacks at least, i.e. internal layer and at least one skin that links to each other with internal layer.Preferably, this multi-layered tissue paper comprises the layer of three stacks, and promptly in one or intermediate layer and two skins, internal layer is between two skins.Two skins preferably mainly contain the fibre composition of short relatively paper fibre, and its average fiber length is about the 0.5-1.5 millimeter, preferably less than about 1.0 millimeters.These short paper fibres are broad-leaved wood fiber normally, preferred leaf wood kraft fibers, and the fiber that is most preferably obtained by eucalyptus.Internal layer preferably mainly contains the fibre composition of long relatively paper fibre, and its average fiber length is at least about 2.0 millimeters.These long paper fibres are needle-leaved wood fibre normally, preferred northern needlebush kraft fibers.Preferably, most of particulate filler of the present invention is included at least one skin of the multi-layered tissue paper width of cloth of the present invention.More preferably, most of particulate filler of the present invention is included in two skins.

But creped tissue paper product monolithic tissue paper product or the multi-ply tissue paper product made by the single or multiple lift creped tissue paper width of cloth.

Making the method and apparatus of paper web knows those of ordinary skills.In a typical method, in the pressurization head box, provide the low concentration intermittent pulp proportioning.Head box has an opening, is used to carry the skim intermittent pulp proportioning to be deposited on fourdrinier wire, to form wet web.Then by vacuum dehydration, usually with the fibre concentration of this paper web dehydration to about 7%-25% (heavily being as the criterion) with total paper web.

According to being disclosed in method of the present invention,, moisture papermaking batching is deposited on the porose surface, to form initial paper web for preparation adds the tissue paper product of filling out.Scope of the present invention also comprises the tissue paper product that is produced by the shaping of multiple ply dheet, wherein two-layer or multilayer batching preferably by as the deposition of the materials flow separately of the fibrous suspension of dilution in the multichannel head box form.Each layer is preferably by dissimilar fibrous, and these fibers generally are long relatively needlebush and relative short broad-leaved wood fibers, as used in the multi-layered tissue paper manufacturing.If each layer is initial is in the online formation that separates, and so thereafter at hygrometric state, each layer meeting is combined together to form multi-layered tissue paper.These paper fibres are generally long relatively needlebush and relative broad-leaved wood fiber of lacking preferably by dissimilar fibrous.More preferably, in said paper fibre, it is about 50% that broad-leaved wood fiber accounts at least, and said needle-leaved wood fibre accounts for about 10% at least.

Make according to the papermaking process of filling out tissue paper product that adds of the present invention being used for, comprise paper web is transferred to blanket or fabric felt, the step of the tissue paper of common as known in the art blanket squeezing also clearly comprises within the scope of the invention.In this step, by with web transfers to dewatering woollen blanket and squeeze paper web, by the squeezing operation water is entered the blanket from paper web and dewaters, wherein paper web is subjected to the pressure that produced by relative mechanical part such as cylinder roller.Owing to make the paper web dehydration need significant pressure by this way, therefore the final paper web of being made by common blanket squeezing has high relatively tightness, and its characteristics are to have uniform tightness in whole paper web structure.

Make according to the papermaking process of filling out tissue paper product that adds of the present invention being used for, comprise the step of half-dried paper web being transferred to Flying Dutchman, during transferring to the cylindrical steam roller bench that this area is called Flying Dutchman, paper web is squeezed.This transfer is to work as the cylindrical relatively roller of pressing to paper web by mechanical means.When paper web is pressed towards the Yankee surface, also vacuum can be used for paper web.Also can use a plurality of Flying Dutchman rollers.

The papermaking process that preferred manufacturing adds the variation of filling out tissue paper comprises so-called pattern densifying method, and wherein the characteristics of page final structure are to have the relative high bulk district and a series of densification districts that are dispersed in the relative high fiber tightness in the high bulk district of low relatively fiber tightness.In addition, high bulky district is also referred to as occipital region (pillow regions).The dense area is also referred to as presses joint district (knuckle regions).The dense area can separate each other in high bulky district discontinuously, perhaps can connect in high bulky district or fully or partly.The zone of preferred higher tightness is continuous, and the high bulk district is discontinuous.The preferable production process of the tissue webs of pattern densification is disclosed in the US3 of Sanford and Sisson, 301,746 (on January 31st, 1967 issued), the US3 of Peter G.Ayers, 974,025 (on August 10th, 1976 issued), the US4 of Paul D.Trokhan, 191,609 (on March 4th, 1980 issued), the US4 of Paul D.Trokhan, 637,859 (on January 20th, 1981 issued), people's such as Wendt US4942077 (issue July 7 nineteen ninety) is among people's such as people's such as Hyland European Patent Publication No No.0617164A1 (on September 28th, 1994 is open) and Hermans the European Patent Publication No 0616074A1 (on September 21st, 1994); All these documents all are hereby incorporated by.

For forming pattern densification paper web, behind sheet forming, immediately paper web is transferred to forming fabric rather than woollen blanket.This paper web is comprised row's support and putting of forming fabric relatively, the relative row's support of this paper web is squeezed, thus, the position of corresponding contact point between row's support and wet web produces the dense area in paper web.In this operation, do not have the remainder of compressed paper web to be called as high bulky district.By using hydraulic pressure, as vacuum plant or blow through drier, this high bulky district can also be subtracted close further.By this way this paper web is dewatered or dispensable predrying, so that avoid the compression in high bulky district basically.This can preferably pass through hydraulic pressure, as utilizes vacuum plant or blow through drier, or finishes by paper web is carried out mechanical compress with respect to row's support on the other hand, and wherein high bulky district is not compressed.Can be with dehydrating operations, the shaping operation of dispensable predrying operation and dense area combination or partly combination are to reduce the total treatment step that is carried out.The moisture of transferring to the half-dried paper web of Flying Dutchman surface is less than about 40%, and forced hot air is by illustrated half-dried paper web, and half-dried paper web forms low tightness structure on said forming fabric simultaneously.

Pattern densification paper web is transferred to Flying Dutchman and bone dry, preferably still avoid mechanical expression.The creped tissue paper surface of preferred about 8%-55% comprises the fine and close joint (knuckle) of pressing, and it has the relative firmness that is at least high bulky district tightness 125%.

This row's support preferably has the joint of pressure composition and arranges embossed carrier fabric (imprinting carrierfabric), and this pressure joint plays a part support, and it will help under working pressure, form the dense area.Press the pattern of joint to constitute this row's support that before is called as the embossed carrier fabric, it is disclosed in the US3 of Sanford and Sisson, 301,746 (on January 31st, 1967 issued); Salvucci, people's such as Jr US3,821,068 (on May 21st, 1974 issued), the US3 of Ayers, 974,025 (on August 10th, 1976 issued), people's such as Friedberg US3,573,164 (on March 30th, 1971 issued), the US3 of Amneus, 473,576 (on October 21st, 1969 issued), the US4 of Trokhan, the US4 of 239,065 (on December 16th, 1980 issued) and Trokhan, in 528,239 (on July 9th, 1985 issued), all these are hereby incorporated by.

Most preferably, hydraulic pressure is put on paper web, make initial paper web can be adapted to the surface of the unlimited drying/impression fabric of mesh, and after this, hang down tightness page manufacture process as part, heat is predrying on said fabric.

The manufacturing step that is included in another variation in the present invention comprises the multi-layered tissue paper structure that forms so-called uncompacted no fine and close pattern, this is described in Joseph L.Salvucci, Jr. with the US3 of Peter N.Yiannos, 812,000 (on May 21st, 1974 issued), Henry E.Becker, the US4 of Albert L.McConnell and Richard Schutte, in 208,459 (on June 17th, 1980 issued), these two pieces of patents are hereby incorporated by.Usually, the tissue paper structures of the one-tenth multilayer of uncompacted, no fine and close pattern is to make in the following way: be deposited on the papermaking batching on the forming net with holes as on the fourdrinier wire with the formation wet web; Has at least 80% fibre concentration up to this paper web with this paper web drainage and there not being to remove under the mechanical expression additional moisture content; And it is this paper web is wrinkling.Remove from paper web by vacuum dehydration and heated drying and to anhydrate.The structure that generates is soft but the high bulking paper page or leaf of the intensity difference of compacting fiber not relatively.Binding material preferably adds to the paper web part before wrinkling.

The advantage relevant with implementing the present invention comprises can reduce the needed paper fibre amount of specified rate tissue paper product of producing.And, the optical property of tissue paper product, particularly opacity also is improved.These advantages have intensity values and be hang down the hair tissue webs in obtained realization.

Just as used herein, term " opacity " refers to the anti-light transmission of tissue webs, and this light has and the corresponding to wavelength of the visible part of electromagnetic spectrum.This " than opacity " is per 1 gram/rice (specificopacity) ²Measuring of the opacity that quantitative tissue webs is given.Measuring opacity and calculate will be in the aft section detailed description of this specification than the method for opacity.Preferably have ratio opacity according to tissue webs of the present invention greater than about 5%, more preferably greater than about 5.5%, and most preferably greater than about 6%.

Just as used herein, term " intensity " refers to the total tensile strength of unit (specific total tensilestrength), and this definite method of measuring is included in the aft section of this specification.This tissue webs according to the present invention is high-intensity.Being generally of their the total tensile strength of unit is at least about 0.25 meter, more preferably greater than about 0.40 meter.

Term " fall hair " and " dry linting " here are used interchangeably, and are meant that when measuring in controlled friction testing instrument, tissue webs discharges the tendency of fiber or particulate filler, and this method of testing will be in the aft section detailed description of this specification.It is relevant with intensity with dry linting to fall hair, goes into degree in the structure because the tendency of release fiber or particulate is directly connected to this fiber or particle set.When total set value increases, intensity will increase.Yet, having the acceptable strength of thinking value but have and unacceptablely fall hair or the dry linting value is possible, this is because fall hair or dry linting can be limited to the part.For example, the surface of tissue webs can be easy to hair or dry linting, but subsurface combination degree can be enough to make total intensity level to bring up to complete acceptable value simultaneously.In another situation, this intensity can obtain from the framework of long relatively paper fibre, and fiber fines or particulate filler are not enough to be combined in the structure.According to of the present invention add fill out tissue webs be hang down relatively the hair.Preferably be lower than about 12 the gross value that falls,, and most preferably be lower than 8 more preferably less than about 10.

Multi-layered tissue paper of the present invention needing can be used for any occasion of softness, absorbefacient multi-layered tissue paper products.The useful especially purposes of multi-layered tissue paper of the present invention is toilet paper and facial tissue product.Monolithic and multi-ply tissue paper product all can be produced by paper web of the present invention.

Analyze and method of testing A. tightness

The tightness of term multi-layered tissue paper is the average tightness that quantitatively goes out divided by THICKNESS CALCULATION by paper as used herein, and carries out suitable unit conversion.The thickness of multi-layered tissue paper is when standing the 95g/ inch as used herein ²(15.5g/cm ²) thickness of paper during compression load.B. the mensuration of molecular weight

The main distinction feature of polymeric material is their molecular size.Performance that polymer is used for different purposes is almost completely obtained by their macromoleculariness matter.For these materials are described fully, be essential to the method that has some to determine and to measure their molecular weight and molecular weight distribution.Use term " relative molecular mass " more more accurate, but the latter is more commonly used in polymer technology than " molecular weight ".In fact not determining molecular weight distribution always.Yet, using chromatographic technique, this will become more commonly used.On the contrary, represent molecular size by the molar mass average value.Mean molecule quantity

If we consider simple molecular weight distribution [its expression has the molecular wt percentage (Wi) of relative molecular mass (Mi)], determine that so some useful mean values are possible.With the molecular amounts (Ni) of specific size (Mi) is that benchmark is averaged and obtained number-average molecular weight.

Mn = \frac{ΣNiMi}{ΣNi}

The important results of this definition is, is the Avogadro number that the number-average molecular weight of unit comprises molecule with the gram.This definition of molecular weight is consistent with the definition that single dispersing molecule kind promptly has the molecule of same molecular amount.The more significant meaning of this definition is, if the molecular number of the polydisperse polymer, non uniform of given quality can be measured with certain method, so just can easily calculate Mn.This is the colligative property based measurement.

With the weight percent (Wi) of the molecule of given quality (Mi) serves as to average and obtain the definition of weight average molecular weight in the basis

Mw = \frac{ΣWiNi}{ΣWi} = \frac{ΣNiM i^{2}}{ΣNiMi}

Mw is the means of the expression polymer molecular weight more useful than Mn, and this is because it reflects melt viscosity and mechanical performance as polymer more accurately, and therefore is used for the present invention.C. the mensuration of packing material size

Particle diameter is a key factor determining carrier performance, particularly when it relates to when making filler keep ability in the page.Clay particle particularly, it is thin slice or bulk, rather than spherical, can be used as the not fixing relative measurement of particle of shape but be called measuring of " quite sphere diameter ", and this is one of main method of industrial mensuration clay and other particulate filler particle diameter.The available TAPP1 practical approach 655 of the mensuration of the suitable sphere diameter of filler is carried out, and this method is based on Sedigraph ^Analytic approach is promptly by measuring from such instrument that Georgia State NorCross city Micromeritics instrument company (Micromeritics InstrumentCorporation) bought.This instrument is a gravitational settling speed of measuring the dispersion suspension liquid of particulate filler with soft X-ray, and uses the Stokes law to calculate suitable sphere diameter.

D. the quantitative analysis of filler in the paper

The those of ordinary skill in ability city will recognize have many methods can carry out the quantitative analysis of non-cellulose filler material in the paper.For helping enforcement of the present invention, will two kinds of methods that be suitable for most preferred inorganic type filler be described in detail.First method, ashing generally is suitable for inorganic filler.Second method is to measure kaolin by XRF, and it is particularly suitable for the filler of particularly suitable in the invention process, i.e. kaolin.

Ashing

Ashing is carried out with Muffle furnace.In this method, at first to clean precision balance (four placebalance), demarcate and calibration.Then, on the dish of precision balance, weigh up clean, empty platinum dish weight.With the gram is the weight (being accurate to 0.01 gram) of empty platinum dish under the unit record.In re-graduation sky not at ordinary times, being nearly adding of 10 grams fills out the tissue paper sample and puts into the platinum dish after carefully folding.With the gram weight (being accurate to 0.01 gram) of platinum dish and paper under the unit record.

Then, at low temperatures with the paper in the pre-ashing platinum of the Bunsen flame dish.Must be when doing this work carefully to avoid gas to carry the formation of ash (air-borne ash).Carry ash if observed gas, must prepare new sample so.After the fray-out of flame by pre-cineration step generation, sample is put into Muffle furnace.Muffle furnace should be 575 ℃ temperature.Make sample fully nearly 4 hours of ashing in Muffle furnace.After 4 hours, sample is taken out and is placed on clean, the anti-surface of firing with thong.Make sample cooling 30 minutes.After the cooling, be the weight (being accurate to 0.01 gram) that unit weighs up platinum dish/ash content composition with the gram.Write down this weight.

From the weight of platinum dish/ash content composition, deduct the weight of clean, empty platinum dish, just can calculate and add the content of ashes of filling out in the tissue paper.With the gram is that unit writes down this content of ashes weight (being accurate to 0.01 gram).

Filler loss during by the understanding ashing (as because the water vapour loss in the kaolin) can be converted into filler weight with content of ashes weight.Filler loss when measuring ashing at first weighs up the weight of clean, empty platinum dish on the dish of precision balance.With the gram is the weight (being accurate to 0.01 gram) of empty platinum dish under the unit record.In re-graduation sky not at ordinary times, the fillers that carefully are nearly 3 grams are poured the platinum dish into.With the gram is the weight (accurate 0.01 gram) of platinum dish/fill composition under the unit record.

Then this sample is carefully put into and be in 575 ℃ Muffle furnace.Make sample fully nearly 4 hours of ashing in Muffle furnace.After 4 hours, sample is taken out and is placed on clean, the anti-surface of firing with belt (thong).Make sample cooling 30 minutes.After the cooling, be the weight (being accurate to 0.01 gram) that unit weighs up platinum dish/ash content composition, write down this weight with the gram.

Calculate the ashing percentageloss of original packing samples with following equation:

Kaolinic ashing percentageloss is 10-15%.Available then following equation will be that the original ash content weight of unit is converted into the gram with the gram is the filler weight of unit:

Available then following equation calculates the original filer content percentage of filling out in the tissue paper that adds: Measure kaolin by XRF

Come compared with the Muffle furnace ashing method, the major advantage of XRF method is that speed is fast, but it is not generally to be suitable for.Compare with the time that the Muffle furnace ashing method is used, the XRF spectrometer can be in 5 minutes the kaolin amount in the quantitative assay paper delivery sample.

The x-ray fluorescence method is based on institute's working sample and uses from the bombardment of the X-ray photons in X-ray tube source.The bombardment that is produced by high-energy photon can make the nuclear energy level electronics be subjected to by the caused photoelectron emissions of element that is present in the sample.These empty nuclear energy levels are filled by outer-shell electron then.Thisly can produce fluorescence process, so that the element that extra X-ray photons can be present in the sample is launched by the filling that outer-shell electron carried out.For these x-ray fluorescence transition, each element all has distinct " impression of the hand " (fingerprint) energy.The available silicon semiconductor detector that oozes lithium of the identification of these elements of this energy and emission x-ray fluorescence photon to be determined is measured.This detector makes the energy of measuring the impact photon become possibility, and therefore can discern the element that is present in the sample.In most of sample matrices, all can discern the element from sodium to uranium.

With regard to the kaolin filler, the element that survey is silicon and aluminium.The specific x-ray fluorescence instrument that is used for the clay analysis is the Spectrace 5000 by the Baker-Hughes company manufacturing of California Mountain View.The first step of clay quantitative analysis is to add with the known clay of a cover to fill out the tissue paper standard sample as being that the tissue paper of 8-20% is calibrated this instrument with clay content.

The available above-described Muffle furnace ashing method of accurate clay amount in these reference sheets is measured.As one of reference sheet, in blank pattern is also included within.At least to calibrate this instrument with five reference sheets that comprise desired target kaolin value.

Before the actual alignment process, the power of X-ray tube is adjusted to 13 kilovolts and 0.20 milliampere.Set this instrument and carry out integration being contained in the aluminium in the clay and the detectable signal of silicon.At first pattern is cut into 2 inches * 4 inches (paper slips of 5.08cm * 10.16cm).Then this paper slip is folded into 2 inches * 2 inches (5.08cm * 5.08cm), make away from drying cylinder side paper web outside.This pattern is put on the top of pattern cup and is fixed in place with clasp.During the preparation pattern, must be careful, lie on the top of pattern cup to keep pattern.Calibrate this instrument with the known standard of this cover then.

After having calibrated instrument, linear calibration curve is stored in the internal memory of computer system with the known standard sample of this cover.This linear calibration curve can be used for calculating the clay amount in the unknown pattern.For guaranteeing the stable of x-ray fluorescence system and work correctly that the inspection sample of a known clay content is followed the unknown sample operation of every cover.Produced incorrect result (clay content known with it differs 10-15%) if check the analysis of sample, this appliance requires carries out trouble shooting and/or recalibration so.

For each Papermaking Conditions, to measure 3 clay contents in the unknown sample at least.Write down the mean value and the standard deviation of these three kinds of patterns.If the using method of clay is doubtful or have a mind to set up new method to change the clay content among page horizontal (CD) or vertical (MD), more pattern need laterally or vertically measured so.E. tissue paper falls the mensuration of hair

Gross weight and can measure by what tissue paper product produced with Sutherland friction testing instrument.This tester uses motor-driven, the blanket 5 times of friction-loaded on fixing toilet paper.Before and after friction testing, measure Hunter color L value.Calculate the poor of these two Hunter color L values, with this as falling gross value.The pattern preparation

Before falling mao friction testing, should handle pattern to be measured according to Tappi method #T402OM-88.Here, pattern will be in the temperature range of the rh value of 10-35% and 22-40 ℃ preliminary treatment 24 hours.After the preliminary treatment, pattern should be handled 24 hours in the temperature range of the relative humidity of 40-52% and 22-24 ℃.Friction testing also should carry out in that constant temperature and humidity is indoor.

Sutherland friction testing instrument can obtain from test mechanical company (Testing Machines) (New York Amityville 11701).When this tissue paper of preparation, any product that may have been rubbed in the time of at first will getting rid of with waste treatment is as the paper roll outside manufacture.For the multi-disc finished paper, get three patterns (each pattern contains the two sheets of paper of multi-disc product), and receive on the experimental bench.For the monolithic product, get six patterns (each pattern contains the two sheets of paper of monolithic product).And be placed on the experimental bench.Then each pattern is carried out folded in half, so that folding line is horizontal (CD) generation along the tissue paper sample.For the multi-disc product, guarantee that the outside face in the folding back of outside one side and pattern is identical.In other words, not tearing the scraps of paper is separated from each other it and opposed facing of friction testing product the inside.For the monolithic product, make 3 patterns, away from outside the drying cylinder side course and 3 patterns, outside the Flying Dutchman side course.The outer pattern of record Yankee side course and away from the outer pattern of Yankee side course.

Obtain 1 30 inches * 40 inches (the Crescent#300 presspapers of 76.2cm * 101.6cm) from Cordage company (No. 800, E.Ross road, the city of Cincinnati, Ohio, postcode 45217).Use paper cutter, cut out 6 areas and be 2.5 inches * 6 inches (presspapers of 6.35cm * 15.24cm).Presspaper is placed on the fixing pin of Sutherland friction testing instrument, on each piece of six blocks of presspapers, makes a call to two holes.

If test monolithic finished paper product, also (6.35cm * 15.24cm) presspaper is put on 6 folding patterns of front centring with 2.5 inches * 6 inches of each pieces carefully so.6 inches wide that guarantee presspaper is parallel with vertical (MD) of each tissue paper sample.If test multi-disc finished paper product so only needs 3 2.5 inches * 6 inches (presspapers of 6.35cm * 15.24cm).Centring also is put into each piece presspaper on 3 folding patterns of front carefully.And 6 inches wide of will guarantee presspaper are parallel with vertical (MD) of each tissue paper sample.

One side of the expose portion of tissue paper sample is folded on the back side of presspaper.With (3/4 inch wide Scotch board, St.Paul is on one side the adhesive tape that MN) obtains is fixed to this on presspaper from 3M company.Catch other to stretch out tissue paper limit outside the presspaper carefully, and nattily it is folded on the back side of presspaper.When making page be fixed to cardboard nattily, second limit is fixed to the back side of presspaper with adhesive tape.Each pattern is repeated this step.

Each pattern is turned over, and the blended rubber band is fixed to the widthwise edge of tissue paper on the presspaper.Half of adhesive tape should contact with tissue paper and second half adheres on the presspaper.Each pattern is repeated this step.If the tissue paper sample ruptures, tears or any moment during this pattern preparation process galls, abandoned well is manufactured new pattern with new tissue paper bar so.

If test multi-disc product processed will have 3 patterns so on presspaper.For the monolithic finished paper, will have so 3 away from the outer pattern of drying cylinder side course on cardboard and the pattern outside 3 drying cylinder side courses on cardboard.The woollen blanket preparation:

From Cordage company (No. 800, E.Ross road, the city of Cincinnati, Ohio, postcode: 45217) obtain one 30 inches * 40 inches (the Crescent#300 presspapers of 76.2cm * 101.6cm).Use paper cutter, cut out 6 areas and be 2.25 inches * 7.25 inches (presspapers of 5.72cm * 18.42cm).On the fine flour of presspaper, two in most of edges picture is parallel to the line on short size limit and extends 1.125 inches (2.86cm) from the upper and lower.As lead, inscribe the length trace of line with straight flange carefully with razor blade.Width of nick is half of page thickness.This indentation makes presspaper/blanket fit tightly under the weight of Sutherland friction testing instrument.On the indentation face of presspaper, draw an arrow that is parallel to the long size of presspaper limit.

Cutting 6 blocks long-pending is 2.25 inches * 8.5 inches * 0.0625 inch (tapetum nigrum of 5.72cm * 21.6cm * 0.16cm) (F55 or suitable thing can be buied CT state, No. 550, BristolBroad street, postcode 06010 from New England Gasket company).This blanket is put into green top of presspaper end indentation so that the long limit of blanket and presspaper is parallel and in line.The villous surface of guaranteeing blanket makes progress.About 0.5 inch blanket is stretched out outside most of edges, presspaper upper and lower.The blanket limit that to stretch out with Scotch board adhesive tape is folded on the back side of presspaper nattily.Preparation is 6 blocks of this blanket/presspapers altogether.

For obtaining best repeatability, all patterns all should use with batch woollen blanket and experimentize.Obviously, the situation that also has other a collection of woollen blanket to use up fully.Under the situation that must obtain new a collection of woollen blanket,, determine correction factor to new a collection of woollen blanket.For representational indivedual tissue paper samples and the enough woollen blankets determining correction factor, obtain to measure think that new batch is manufactured 24 presspapers/woollen blanket sample with old batch of woollen blanket.

As following described, before carrying out any friction, in 24 presspapers/woollen blanket sample of new and old batch of woollen blanket each obtains Hunter L reading.Calculate 24 the presspaper/blanket samples and the new mean value of criticizing 24 presspapers/woollen blanket sample of woollen blanket of old batch of woollen blanket.

Then, 24 presspapers/woollen blanket plate that friction testing is newly criticized and 24 presspapers/woollen blanket plate of old batch are as following described.The pattern of each sample of guaranteeing to be used for 24 samples of old and new batch woollen blanket is from batch tissue paper.In addition, when preparation presspaper/tissue paper sample, must carry out the sampling of paper, cause new batch woollen blanket and old batch of woollen blanket more can be as representative tissue paper.Concerning 1 tissue paper product, discarded any product that may be damaged or wear and tear.Then, obtain 48 tissue papers (also claiming page), each has two available unit head.First is had the left side that the long paper slip of two available units is placed on experimental bench, and last is placed on the right of experimental bench in 48 patterns.Mark in the corner of 1 centimetre of area of 1 cm x of the pattern on the experimental bench left side with number " 1 ".Continued labelling residue pattern, mark to 48 successively, the number that causes last pattern on the experimental bench right side is 48.

The pattern of 24 odd numbered is used for new blanket, and the pattern of 24 even numbers is used for old blanket.Successively the odd numbered pattern is arranged to the highest from minimum.Arrange to the highest number of dual numbers successively pattern from minimum.Now, the minimum number of every group of pattern is marked, the second high number is marked with letter " O " with letter " Y ".With the low sample of this " Y " that replaces/" O " form continued labelling.With " Y " pattern the outer page of Yankee side course is fallen hair analysis, and the page away from Yankee side layer is fallen hair analysis with " O " pattern.For 1 flake products, now always have 24 new batch woollen blanket and old batch of woollen blanket patterns.In these 24 patterns, 12 be used for the outer page of Yankee side course fall hair analysis, and 12 are used for falling hair analysis away from the outer page of Yankee side course.

All 24 Geju City blanket patterns are rubbed and measure Hunter colourity L value, as following described.Write down the Hunter colourity L value of 12 Yankee side patterns of old blanket.Calculate the mean value of these 12 values.Write down 12 Hunter colourity L values of old blanket away from Yankee side pattern.Calculate the mean value of these 12 values.From the average Hunter colourity L value of Yankee side friction pattern, deduct the average Hunter colourity L value of the blanket that the beginning and end are rubbed, the Δ mean difference of Here it is Yankee side pattern.Deduct the average Hunter colourity L value of the blanket that the beginning and end are rubbed from the average Hunter colourity L value away from Yankee side friction pattern, Here it is away from the Δ mean difference of Yankee side pattern.Calculate Yankee side Δ mean difference and away from the summation of Yankee side Δ mean difference and divided by 2.Here it is the uncorrected gross value that falls for old blanket.If a general old blanket blanket correction factor is arranged, so just it can be added to uncorrected old blanket and fall in the gross value.This value is exactly that the old blanket of proofreading and correct falls gross value.

All 24 new blanket patterns are rubbed and measure Hunter colourity L value, as following described.Write down the Hunter colourity L value of 12 Yankee side patterns of new blanket.Calculate the mean value of these 12 values.Write down 12 Hunter colourity L values of new blanket away from Yankee side pattern.Calculate the mean value of these 12 values.From the average Hunter colourity L value of Yankee side friction pattern, deduct the average Hunter colourity L value of the blanket that the beginning and end are rubbed.The Δ mean difference of Here it is Yankee side pattern.Deduct the average Hunter colourity L value of the blanket that the beginning and end are rubbed from the average Hunter colourity L value away from Yankee side friction pattern, Here it is away from the Δ mean difference of Yankee side pattern.Calculate Yankee side Δ mean difference and away from the summation of Yankee side Δ mean difference, and divided by 2.Here it is, and uncorrected new blanket falls gross value.

The old blanket of writing down correction falls gross value and uncorrected new blanket falls the poor of gross value, and this difference is newly to criticize the blanket correction factor of blanket.

Gross value is fallen in the correction that should equal old blanket in the gross value of not proofreading and correct that this blanket correction factor is added to new blanket.

The step of same type also is suitable for the biplate tissue paper product, and 24 patterns are tested with old blanket, and 24 patterns are tested with new blanket.But only the skin to the used multi-disc product of consumer carries out friction test.As noted above, guarantee the meticulous preparation of pattern, think that old and new blanket obtains representational pattern.The maintenance of 4 pound weight things

This 4 pound weight thing has effective contact zone of 4 square inches, has produced 1 pound/square inch contact pressure.Because by changing the friction pad regulative contact pressure on the weight surface, therefore, it is very important only using the friction pad of a tame manufacturer (machinery service department of Kalamazoo city, M1 state Brown company) supply.If these fill up hardening, wear and tear or fall slag, must change so.

Not the time spent, this weight must be placed on the fixed position, causes friction pad can not support the whole weight of weight.Preferably weight is placed on the next door of pad.The calibration of friction testing instrument:

Must calibrate Sutherland friction testing instrument before using.At first, the switch of tester is turned to " cont " position, open Sutherland friction testing instrument.When the tester arm is in the most close user's position, the switch of tester is turned to " auto " position.Pointer arm on the high range dish is moved on to location, " 5 " position, tester is set reciprocal 5 times.Make a round trip be weight backward and once complete forward motion.When beginning of testing each time and end, the end of friction block all should be in the position nearest with the operator.

As described above, on the presspaper sample, prepare a tissue paper.In addition, as described above, on the presspaper sample, prepare a woollen blanket.These two samples will be used for the calibration of instrument, and will not obtain data as actual sample.

By on fixing pin, slipping over the hole in the cardboard, calibration tissue paper sample is placed on the substrate of tester.Fixing pin can be avoided the test period movement of sample.To calibrate blanket/presspaper sample and be fixed on the 4 pound weight things, the presspaper face is contacted with the weight pad.Guarantee that presspaper/blanket composition is entirely pasting weight.This weight is suspended on the tester arm, and with the tissue paper sample be placed on lightly weight/woollen blanket composition below.The weight end nearest with the operator must be not on tissue paper sample body on the presspaper of tissue paper sample.Woollen blanket must keep smooth placement on the tissue paper sample, and is 100% contact with tissue paper surface.Depress " push " button, start tester.

Meter is reciprocal number of times down, and the start and stop bit of observation and the record blanket covering weight relevant with pattern is put.If reciprocal sum is 5, and if the end that covers weight with the nearest blanket of operator be to be in above the tissue paper sample during in the test beginning with at EOT, tester is prepared to use through calibration so.If be not if that 5 times or the end that covers weight with the nearest blanket of operator are in the test beginning or be to be in above the tissue paper sample of reality when finishing toward negative total, repeat this calibration steps so, up to 5 times back and forth after, till the end that covers weight with the nearest blanket of operator all is in above the presspaper in the beginning of test with when finishing.

In the actual test process of sample, monitoring and observation reciprocal time and blanket cover the starting point and the halt of weight.In case of necessity, calibrate again.The calibration of HUNTER chromascope:

According to the step of being summarized in this instrumentation handbook, the Hunter colour difference instrument of black and white on-gauge plate is proofreaied and correct.If does not also do these in the past 8 hours, to carry out also that standardized stability is checked and the chromaticity stability inspection of every day.In addition, must check zero albedo (zeroreflectance), and if necessary, proofread and correct again.

White on-gauge plate is placed on the sample stage under the instrument mouth.Decontrol sample stage, and sample panel is elevated under the setting-out product position.

Use " L-Y ", " a-x " and " b-z " calibration knob, the adjusting instrument is read in turn and is pressed " L ", during " a " and " b " button, " L " of standard white plate, " a " and " b " value.The mensuration of sample

The fixed first step is to measure the Hunter chromatic value of tapetum nigrum/presspaper sample to fall full scale, and this carried out before being rubbed on the toilet paper at it.The first step of this mensuration is the height of blank of debasing the standard below the instrument mouth of Hunter chromascope.Aim at the center that blanket covers presspaper, simultaneously the back side of the colorimeter of pointed on on-gauge plate.Decontrol sample stage, make blanket cover presspaper and be elevated under the setting-out product position.

Because therefore the wide check district diameter that only is slightly larger than of blanket will guarantee that blanket covers the check district fully.After confirming covering fully, depress the L button and wait for stable reading.Read and write down this L value (being accurate to 0.1 unit).

As use the D25D2A head, reduce blanket so and cover presspaper and on-gauge plate, with the presspaper half-twist of blanket covering, so that the right of pointed colorimeter.Then, decontrol sample stage, and check once more to guarantee that the check district covers with blanket fully.Depress the L button.Read and write down this value (being accurate to 0.1 unit).For the D25D2M instrument, the value of record is a Hunter colourity L value.For the D25D2A head, also write down the sample reading of rotation here, therefore, Hunter colourity L value is the mean value of two record values.

Use this method that all blankets are covered the mensuration that presspaper carries out Hunter colourity L value.If Hunter colourity L value all within 0.3 unit, is averaged, to obtain initial L reading mutually so.If Hunter colourity L value not within 0.3 unit, is discarded those not blanket/presspapers in this scope so.Prepare new sample and repeat Hunter colourity L pH-value determination pH, up to the Hunter of all samples colourity L value mutually all within 0.3 unit difference.

For the mensuration of the tissue paper/presspaper of reality, on fixing pin, slip over the hole in the cardboard and tissue paper sample/presspaper is placed on the substrate of tester.Fixing pin can be avoided the test period movement of sample.To calibrate blanket/presspaper sample and be fixed on the 4 pound weight things, the presspaper face is contacted with the pad of weight.Guarantee that presspaper/blanket is entirely pasting weight.This weight is suspended on the tester arm, and with the tissue paper sample be placed on lightly weight/woollen blanket below.The weight end nearest with the operator must be not on tissue paper sample body on the presspaper of tissue paper sample.It is smooth that woollen blanket must keep on the tissue paper sample, and be 100% contact with tissue paper surface.

Then, depress " Push " button, start tester.After reciprocal 5 times, tester will stop automatically.The record blanket covers the stop position of the relative pattern of weight.If covering the end of weight towards operator's blanket is on presspaper, tester is in correct duty so.If the end that covers weight towards operator's blanket stops this mensuration so, and according to pointed method in the top Sutherland friction testing instrument calibrated section instrument is recalibrated on pattern.

Remove and have the weight that blanket covers presspaper.Check the tissue paper sample.Tear as pattern, then discarded this blanket and tissue paper, and restart.If the tissue paper sample is undamaged, remove the presspaper that blanket covers from weight so.Measure described method according to top for blank blanket, measure the Hunter colourity L value on the blanket covering presspaper.The Hunter colourity L value of record friction back blanket.Rub, measure and write down the Hunter colourity L value of all remaining samples.

After all tissue papers have all been measured, remove and discarded all woollen blankets.Do not re-use the blanket bar.Use presspaper, up to its bending, tear, soft or when no longer having smooth surface till.Calculate:

From each measured value, deduct not with the average initial L value of blanket, just can obtain Δ L value away from Yankee side pattern and Yankee side pattern.Remember only the rubbed one side of page of multi-disc product.Therefore, for the multi-disc product, obtain three Δ L values.Average to these three Δ L values, and from this last mean value, deduct the blanket factor.This last result be called the 2-flake products fabric side fall gross value.

For the monolithic product, not only obtained the Yankee side but also can obtain measured value away from the Yankee side, each from three Yankee side L values and three deduct the not average initial L value of usefulness blanket away from the Yankee side L value each.Calculate the average delta L value of three Yankee sides.Calculate the average delta L value of three fabric side.From each mean value, deduct the blanket factor.This last result is called that monolithic product fabric side is fallen gross value and the Yankee side is fallen gross value.By calculating the mean value of these two values, what just can obtain whole monolithic product finally falls gross value.F. the mensuration of (specially) group (subjective assessment) pliability of tissue paper

It is desirable to, before pliability is measured, should nurse one's health the pattern that to measure according to Tappi method #T402OM-88.Here, pattern will be in the temperature range of the relative humidity of 10-35% and 22-40 ℃ preliminary treatment 24 hours.After the preliminary treatment, pattern should be handled 24 hours in the relative humidity of 48-52% and 22-24 ℃ of temperature range.

It is desirable to, group measures pliability and should carry out in that constant temperature and humidity is indoor.If impossible, all samples comprises that the contrast pattern all should be under the same environmental conditions and measures.

It is to carry out with the form that is similar to described in the artificial feel detection method (Manual onSensory Testing method) under relatively situation in pairs that pliability is measured, this method is embodied in the ASTM special technique publication 434 of nineteen sixty-eight U.S.'s detection and materials association publication, and it incorporates into own forces in this for reference.Pliability is to adopt the subjectivity that is called paired difference detection (Paired Differene Test) to detect to estimate.This method has been used the external standard of test material.For the sense of touch pliability, provide two patterns so that the tester cannot see pattern, and the tester need select one of them according to the sense of touch pliability.Measurement result is with scoring unit (PSU) of so-called group record.Measure the pliability data of reporting with PSU to obtain here about pliability, need carry out many groups pliability and measure.In each mensuration, ten experienced pliability detection persons are required three compositions are made appraisal to the relative pliability of pattern.Estimated many to pattern over the ground by each detection person each: a pattern of every centering is called X, and another is called Y.In brief, each X pattern is that its paired Y pattern is assessed in the following manner relatively:

1. if be evaluated as may be than the soft point of Y for X, so the grade of X be+1; And if Y be evaluated as may be than the soft point of X, the grade of X is-1 so;

2. if X is be evaluated as really than the soft point of Y, the grade of X is+2 so; And if Y is be evaluated as really than X soft spots, the grade of X is-2 so;

3. if X is be evaluated as soft more much than Y, the grade that gives X so be+3, and if Y be evaluated as softlyer a lot than X, the grade that gives X so is-3; And, last:

4. if X is be evaluated as soft more a lot than Y, the grade that gives X so be+4, and if Y be evaluated as softlyer a lot than X, the grade that gives X so is-4.

These grades are averaged, and come the ecbatic value with PSU unit.Result data is considered to the result that a group is detected.If a pair of above pattern is evaluated, the grade that obtains according to paired statistical analysis comes all are arranged in order to pattern so.Then, on request evaluation of estimate conversion is up or down arranged to obtain one 0 PSU value, this value pattern is selected as 0 benchmark.Determine with respect to the relative grade of 0 benchmark that they have by other pattern then and be the plus or minus value.Group that carry out and average to measure number of times be to make about 0.2PSU represent the notable difference of the soft change of subjective sensation.G. the mensuration of tissue paper opacity

The opacity percentage is measured with Colorquest DP-9000 spectrocolorimeter.Find the on/off switch behind the processor, and open.Made the instrument preheating two hours.If system has entered stand-by state, the arbitrary key on the keypad and make instrument in addition preheating 30 minutes more so.

With filter glass and white ceramic tile instrument is calibrated.The calibration of guaranteeing instrument is to carry out in the mode of reading and according to the explanation that the calibrated section in the DP9000 instrument handbook is given.For calibration DP-9000, press the CAL key on the processor, and carry out according to the prompting shown on the fluorescent screen.You read the reading of filter glass and white ceramic tile under prompting then.

Also must return to zero to DP-9000 according to the explanation that provides in the DP-9000 instrument handbook.Enter the setup mode by the setup key.Limit following parameters: the UF filter: disconnect demonstration: ABSOLUTE reading interval: the identification of single (SINGLE) sample: open or close average: close statistic law: SKIP colour code: XYZ chromaticity index: the SKIP colour difference is marked: SKIP colour difference index: SKIPCMC ratio: SKIPCMC (Commercial) factor: SKIP visualizer: 10 spend light source: DM1 the 2nd light source: SKIP standard: target value: SKIP allowable deviation: SKIP

Confirm that colour code is set to XYZ, visualizer is set to 10 degree, and light source is set to D.A slice pattern is placed on do not calibrate on the white ceramic tile.Also can use the white ceramic tile of calibration.This sample and ceramic tile are risen under the setting-out product position, and definite Y value.

Reduce sample and ceramic tile.Without rotary sample itself, remove white ceramic tile and replace with filter glass.Promote sample and filter glass again and determine the Y value.Guarantee that this 1 tissue paper sample does not rotate between white ceramic tile and filter glass reading.

Calculate the opacity percentage by obtaining the Y reading on the filter glass and the ratio of the Y reading on the white ceramic tile.On duty with this then with 100 fraction values that promptly get opacity.

With regard to this specification, the measured value of opacity is transformed into " than opacity ", in fact this proofreaied and correct the opacity of quantitative variation.Opacity % is transformed into as follows than the formula of opacity %:

Than opacity=(1-(opacity/100) (1/ is quantitative)) * 100,

Here be each gram/rice than opacity unit ²Percentage, opacity unit is a percentage, and quantitative unit is a gram/rice ²

Report the result than opacity and should be accurate to 0.01%.G. the mensuration dry tensile strength of tissue paper intensity

This tensile strength is to measure on one inch wide pattern bar with the anti-tester (Thwing-Albert instrument company, No. 10960, Dutton road, Philadelphia, PA state, postcode 19154) of opening of Thwing-Albert Ihtelect II standard.This method is to prepare to be used on finished paper product, paper roll sample and the unprocessed body paper.Pattern is handled and preparation:

Before the tensile strength test, should handle pattern to be measured according to Tappi method #T402OM-88.Before the test, must be carefully get rid of all plastics from pattern with the carton package material.Pattern should be handled 2 hours in the temperature range of the relative humidity of 48-52% and 22-24 ℃ at least.Pattern preparation and the test of each zeeil tensile strength Z also should be carried out in that constant temperature and humidity is indoor.

For finished paper, the product of discarded any damage.Then, get 5 patterns (also claiming page) with 4 available units, and with one be added to another above, to form long superimposed pattern, the hole between page is overlapped.To be used for the page that machine direction tensile strength measures and put on 1 and 3, and will be used for the page that cross direction tensile strength measures and put on 2 and 4.Then; with paper cutter (JDC-1-10 or JDC-1-12 with safety guard; Thwing-Albert instrument company makes; No. 10960, Dutton road, Philadelphia, PA state; postcode, 19154) cut through the via hole line, to make 4 stacked pattern heaps that separate; also will guarantee to be used for the stacked pattern heap of testing longitudinal and put on 1 and 3, and the stacked pattern heap that is used for transverse test puts on 2 and 4.

Cut two vertical paper slips that 1 inch (2.54cm) is wide from stacked pattern heap 1 and 3.Cut two 1 inch wide horizontal paper slip from stacked pattern heap 2 and 4.Existing 41 inch wide paper slips are used for the machine direction tensile strength test and 41 inch wide paper slips are used for the cross direction tensile strength test.For these finished paper samples, all 81 inch wide paper slips (also claiming page) all are that 5 available units are thick.

For unprocessed body paper and/or paper roll sample; use paper cutter (JDC-1-10 or JDC-1-12 with safety guard; Thwing-Albert instrument company makes; No. 10960, Dutton road, Philadelphia, PA state, postcode 19154) cuts one 8 thick 15 inches * 15 inches (patterns of 38.1cm * 38.1cm) from the mensuration district of pattern.Guarantee that one 15 inches (38.1cm) limits are parallel to vertically and carry out, and being parallel to laterally of another side carried out.Guarantee that pattern handled 2 hours at least in the temperature range of the relative humidity of 48-52% and 22-24 ℃.The test of pattern preparation and each zeeil tensile strength Z also will be carried out in that constant temperature and humidity is indoor.

(pattern of 2.54cm * 17.8cm) is wanted and parallel longitudinal with 7 inches limits of duration to cut 41 inch * 7 inches from 8 15 inches * 15 inches thick preliminary treatment patterns.Write down these patterns as vertical paper roll or unprocessed former pattern.Cut other 41 inch * 7 inches pattern, make 7 inches long (17.8cm) limits simultaneously with laterally parallel.Write down these patterns as horizontal paper roll or unprocessed former pattern.Guarantee that cutting of all fronts all is that (JDC-1-10 or JDC-1-12 with safety guard, Thwing-Albert instrument company makes, No. 10960, Dutton road, Philadelphia, PA state, postcode: 19154) carry out with paper cutter.Now always have 8 patterns: 481 inch * 7 inches thick patterns, its 7 inches limits are parallel to vertically; Article 4,81 inch * 7 inches thick patterns, its 7 inches limits are parallel to laterally.Anti-operation of opening tester

For the practical measurement of tensile strength, be to use anti-tester (Thwing-Albert instrument company, No. 10960, Dutton road, Philadelphia, PA state, the postcode: 19154) opened of Thwing-Albert Intelect II standard.The plane folder is inserted the explanation of being given in this instrument and the operation manual according to Thwing-Albert Intelect II carry out the calibration of instrument.The crossing grip holder speed of instrument is transferred to 4.00 inch per minutes (10.16cm/ branch), and measures length with the 1st and the 2nd and be transferred to 2.00 inches (5.04cm).Break sensitivity should be transferred to 20.0 grams, and pattern is wide should be transferred to 1.00 inches (2.54cm), and pattern is thick should be at 0.025 inch (0.06cm).

Selected dynamometer causes the tensile strength result of the prediction of pattern to be measured to be between 25% and 75% range of dynamometer use.For example, the dynamometer of one 5000 gram can be used for predicting the pattern of tensile strength range between 1250 grams (5000 grams 25%) and 3750 grams (5000 restrain 75%).10% ranges that an anti-tester also can be arranged on 5000 gram dynamometers cause this tester can measure the pattern of prediction tensile strength in 125-375 gram scope.

Get the paper slip of a tensile strength to be measured, the one end is placed in the chuck of an anti-tester, the other end of paper slip is placed in another chuck.The long limit of guaranteeing paper slip is parallel to anti-side of opening tester.To guarantee that also paper slip does not reach outside arbitrary side of two chucks.In addition, the pressure of each chuck must contact with pattern fully.

To test paper slip and put into after two chucks, but monitoring instrument tension force.If it shows 5 gram or higher values, this pattern is too tight so.On the contrary, if after the test beginning and before any numerical value of record,, should test too pine of paper slip so through the 2-3 time of second.

According to the anti-tester of opening of the unlatching described in the anti-tester handbook.After crossing grip holder automatically returned to initial starting position, this test was finished.From instrument calibration dish or digital instrument dash board is that anti-Zhang Zaihe (being accurate to least unit) is read and write down in unit with the gram.

If this instrument can not recover reset condition automatically, carry out necessary adjusting so so that the instrument chuck is got back to its original position.According to described above, next paper slip put into two chucks and be that unit obtains the tensile strength reading with the gram.Obtain the tensile strength reading from the test paper slip.It should be noted that if when testing paper slip should be discarded this reading in chuck or its edge slippage or fracture so.Calculate

For 41 inch (2.54cm) wide finished paper paper slips longitudinally, with these 4 respectively the tensile strength readings of record add up.Remove this summation with the paper slip number of measuring.Paper slip number normally 4.Also to remove the tensile strength summation that is write down with the available units number of each tensile strength paper slip.For 1 and 2 flake products, the available units number is generally 5.

Horizontal finished paper paper slip is repeated this calculating.

For at undressed body paper that vertically cuts or paper roll pattern, 4 tensile strength readings that write down are respectively added up.Summation is divided by the paper slip number of test.This paper slip number is generally 4.Also to remove the tensile strength summation that is write down with the available units number of each tensile strength paper slip.The available units number is generally 8.

Horizontal unprocessed or paper roll sample paper slip is repeated this calculating.

All results are unit with gram/inch (gram per centimeter).

With regard to this specification, this tensile strength should be transformed into " than total tensile strength ", and its definition is with the tensile strength summation of quantitatively removing vertical and horizontal mensuration, and its unit transfers rice to.

Embodiment

The following example is in order to illustrate enforcement of the present invention.These embodiment are with helping description of the invention, but never mean and limit the scope of the invention.The present invention is the restriction of appending claims only.

Embodiment 1

This comparing embodiment has illustrated a reference method, and it does not comprise feature of the present invention.This method illustrates with the following step:

At first, prepare the NSK water slurry of about 3% concentration, and flow to the head box of fourdrinier machine by the slurry pipe with common pulper.

For giving finished paper temporary transient wet strength, prepare the national starch Co-BOND of company 1000 ^1% dispersion, and to be enough to carry %Co-BOND 1000 ^Ratio (based on the dry weight of NSK fiber) it is added in the NSK slurry pipe.By treated suspension is mixed through the on-line mixing device, the absorption of temporary transient wet strengthening resin is strengthened.

At the mixing pump place, with plain boiled water NSK suspension is diluted to about 0.2% concentration.

The water slurry for preparing the eucalyptus fibers of about 3% (by weight) with common pulper.

Eucalyptus fibers suspension is flow to another mixing pump via the slurry pipe, and at this, this suspension has been diluted to about 0.2% concentration with plain boiled water.

The suspension of NSK and eucalyptus fibers flows directly into the suitable multilayer head box of equipping the layering thin plate, so that slurry stream keeps the layer of separation till flowing on the fourdrinier wire of advancing.Use the head box of three Room.The eucalyptus fibers suspension that contains 80% final page dry weight flows directly into and produces two skins in two chambers, and the NSK suspension that accounts for final page dry weight 20% flows directly into produce one deck NSK in the chamber between two eucalyptus fibers floor.In the head box outlet, NSK and eucalyptus fibers suspension mix the compound suspension of generation.

Composite suspension liquid flows on the fourdrinier wire of advancing, and dewaters under the help of deflector and suction flat box.

At the transfer position fibre concentration about 15% o'clock, this initial wet paper web is passed to the shaping blanket with pattern decorative from fourdrinier wire, this shaping blanket is 5-shed open, the satin weave configuration that per inch has vertical 84 and horizontal 76 monofilament respectively, and has about 36% pressure joint (knuckle) district.

Finish further dehydration by the dehydration that vacuum helps, have until paper web till about 28% the fibre concentration.

Keeping with when shaping blanket with pattern decorative contacts, be about 62% (by weight) to fibre concentration with the paper web of pattern decorative is predrying by the hot blast impingement drying.

With the spraying creping adhesives that comprises 0.125% polyvinyl alcohol water solution half-dried paper web is adhered to the Flying Dutchman surface then.Creping adhesives is that the ratio (based on the adhesive solids amount of paper web dry weight) with 0.1% sprays to the Yankee surface.

Paper web is done from Flying Dutchman with doctor blade wrinkling before, the concentration of this fiber is increased to about 96%.

This doctor blade has the oblique angle of about 25 degree, and with respect to the Flying Dutchman device, so that the angle of shock of about 81 degree to be provided.

Make Flying Dutchman with the running of the speed of about 800fpm (feet per minute) (about 244 meters/minute), wrinkling percentage is transferred to about 18%, dried simultaneously paper web forms paper roll with the speed of 656fpm (201 meters/minute).

Paper web is processed into three layers, the wrinkle pattern densification tissue paper product of monolithic, and it quantitatively is about 18 pounds/3000 square feet (0.0029 gram/square centimeters).

Embodiment 2

Present embodiment has illustrated and has added the preparation method who fills out tissue paper that it has shown based on one embodiment of the invention of using cationic flocculant.

The eucalyptus fibers water slurry for preparing about 3% concentration (by weight) with common pulper.Make this suspension through a beater, herein, the freedom of suspension is reduced to about 600 CSF by about 640 CSF (Canadian Standard Freeness).It flows to the paper machine by the delivery of slurry pipe then.

Particulate filler is WW FiL SD ^The kaolin of the trade mark is to be made by the Dry Branch kaolin company of Georgia State Dry Branch.At first, be made into the water slurry that concentration is about 1% solid content by mixing with water.Then by slurry pipe operation, in the slurry pipe, it and cationic starch RediBOND 5327 ^Mix, this starch is to carry with 1% aqueous dispersion form.RediBOND5327 ^Be a kind of waxy corn starch of pre-dispersed type, based on the starch solids addition of the amount of solid of every part of filler, starch is about 0.5% to the ratio of filler.Mix by the on-line mixing device, the absorption of cationic starch is strengthened.This has formed the filler grain suspension of agglomeration.

Then, the filler grain suspension of agglomeration is sneaked into the slurry pipe that is delivering through the eucalyptus fibers of making beating, and with plain boiled water final mixture is diluted to the concentration of about 0.2% (based on the weight of solid packing particle and eucalyptus fibers) at the inlet of mixing pump.After the mixing pump of the mixture that is delivering agglomeration filler grain and eucalyptus fibers, a kind of cationic flocculant Reten 1232 is added in the mixture with the ratio that is equivalent to 0.067% (based on the solid weight of filler and eucalyptus fibers).

Prepare the NSK water slurry of about 3% concentration with common pulper, and flow to the head box of fourdrinier machine via the slurry pipe.

For giving finished paper temporary transient wet strength, prepare the national starch Co-BOND of company 1000 ^1% dispersion, and to be enough to carry 1%Co-BOND 1000 ^Ratio (based on the dry weight of NSK fiber) it is added in the NSK slurry pipe.Mix with treated suspension by the on-line mixing device, the absorption of temporary transient wet strengthening resin is strengthened.

At the mixing pump place, with plain boiled water NSK suspension is diluted to about 0.2% concentration.Behind mixing pump, with a kind of cationic flocculant RETEN 1232 ^Be added in the slurry stream with the ratio that is equivalent to 0.067% (based on the dry weight of NSK fiber).

The suspension of NSK and eucalyptus fibers flows directly into the suitable multilayer head box of equipping the layering thin plate, so that slurry stream keeps the layer of separation till flowing on the fourdrinier wire of advancing.Use the head box of three Room.The eucalyptus fibers and the particulate filler suspension that mix contain the efflux of solids that is enough to obtain 80% final page dry weight.The suspension of this mixing flows directly into the chamber that produces two outer field each floor, and the NSK suspension that contains the efflux of solids that is enough to obtain 20% final page dry weight flows directly into the chamber of the generation one deck between two eucalyptus fibers floor.In the head box outlet, NSK and eucalyptus fibers suspension mix the compound suspension of generation.

At the transfer position fibre concentration about 15% o'clock, this initial wet paper web is passed to the shaping blanket with pattern decorative from fourdrinier wire, and this shaping blanket is that per inch has 5-shed open, the satin weave configuration of vertical 84 and horizontal 76 monofilament respectively and has about 36% pressure joint (Knuckle) district.

With the spraying creping adhesives that contains 0.125% polyvinyl alcohol water solution half-dried paper web is adhered to the Flying Dutchman surface then.Creping adhesives is that the ratio (based on the adhesive solids amount of paper web dry weight) with 0.1% sprays to the Yankee surface.

This doctor blade has the oblique angle of about 20 degree, and with respect to the Flying Dutchman device, so that the angle of shock of about 76 degree to be provided.

Make Flying Dutchman with the running of the speed of about 800fpm (feet per minute) (about 244 meters/minute), wrinkling percentage is transferred to about 18%, dried simultaneously paper web forms paper roll with the speed of 656fpm (200 meters/minute).

Paper web is processed into three layers, monolithic wrinkle pattern densification tissue paper product, and it quantitatively is about 18 pounds/3000 square feet (0.0029 gram/square centimeters).

Embodiment 3

Present embodiment has illustrated and has added the preparation method who fills out tissue paper that it has shown based on second embodiment of the present invention of using Flokal B.

The eucalyptus fibers water slurry for preparing about 3% concentration (by weight) with common pulper.It flows to the paper machine by the delivery of slurry pipe then.

Particulate filler is WW FiL SD ^The kaolin of the trade mark is to be made by the Dry Branch kaolin company of Georgia State Dry Branch.At first, be made into the water slurry that concentration is about 1% solid content by mixing with water, then by slurry pipe operation, in the slurry pipe, it and Flokal B RETEN235 ^Mix, this flocculant is to carry with 0.1% aqueous dispersion form.Based on the amount of the dry weight of the solid weight of flocculant and final finished creped tissue paper product, RETEN235 ^Be to carry to be equivalent to about 0.05% ratio.Mix by the on-line mixing device, the absorption of this flocculant is strengthened.This has formed treated filler grain suspension.

Then, the filler grain suspension of agglomeration is sneaked into the slurry pipe of eucalyptus fibers that is delivering through making beating, and with cationic starch RediBOND 5320 ^Handle final mixture, this starch is to carry with 1% aqueous dispersion form, and is added in the mixture with 0.5% ratio based on the dry weight of the dry weight of starch and final finished creped tissue paper product.Mix by the on-line mixing device, the absorption of cationic starch is strengthened.Then mixing pump the porch final suspension is diluted to the concentration of about 0.2% (based on the weight of solid packing particle and eucalyptus fibers) with plain boiled water.After the mixing pump of the mixture of filler grain that is delivering agglomeration and eucalyptus fibers, a kind of cationic flocculant Microform 2321 is added in the mixture with the ratio that is equivalent to 0.05% (based on the amount of solid of filler and eucalyptus fibers).

At the mixing pump place, with plain boiled water NSK suspension is diluted to about 0.2% concentration.Behind mixing pump, a kind of cationic flocculant Microform 2321 is added in the slurry stream with the ratio that is equivalent to 0.05% (based on the dry weight of NSK fiber).

The suspension of NSK and eucalyptus fibers flows directly into the suitable multilayer head box of equipping the layering thin plate, so that slurry stream keeps the layer of separation till flowing on the fourdrinier wire of advancing.Use the head box of three Room.The eucalyptus fibers and the particulate filler suspension that mix contain the efflux of solids that is enough to obtain final page dry weight 80%, the suspension of this mixing flows directly into the chamber that produces two outer field each floor, and the NSK suspension that contains the efflux of solids that is enough to obtain final page dry weight 20% flows directly into the chamber of the one deck that produces between two eucalyptus fibers floor.In the head box outlet, NSK and eucalyptus fibers suspension mix the compound suspension of generation.

This composite suspension liquid flows on the fourdrinier wire of advancing, and dewaters under the help of deflector and suction flat box.

	Embodiment 1	Embodiment 2	Embodiment 3
	Embodiment 1	Embodiment 2	Embodiment 3	Kaolin content	Do not have	13.3	16.0
Kaolin retention (always)	NA	74	88.6	Kaolin content	Do not have	13.3	16.0
Kaolin retention (always)	NA	74	88.6	Tensile strength (gram/inch)	400	396	407
Compare opacity	5.23	5.84	5.90	Tensile strength (gram/inch)	400	396	407
Compare opacity	5.23	5.84	5.90	Finally fall gross value	7.0	6.9	7.0
Softness values	0.0	+0.02	+0.01	Finally fall gross value	7.0	6.9	7.0

Claims

1. adding of a high strength, softness and low dry linting, filled out tissue paper, it is characterized in that comprising the particulate filler of paper fibre and non-cellulose, said filler accounts for the 5-50% of said tissue paper weight, and described particulate filler is selected from clay, calcium carbonate, titanium dioxide, talcum, alumina silicate, calcium silicates, hibbsite, active carbon, pearl starch, calcium sulfate, glass microballoon, diatomite and composition thereof.

2. adding of claim 1, filled out tissue paper, and wherein said tissue paper has 10-50 gram/rice ²Quantitatively and the 0.03-0.6 gram per centimeter ³Tightness.

3. adding of claim 2, filled out tissue paper, and wherein said tissue paper has 10-30 gram/rice ²Quantitatively and the 0.05-0.2 gram per centimeter ³Tightness.

4. adding of claim 3, filled out tissue paper, and wherein said particulate filler accounts for 8% to 20% of described tissue paper weight.

5. the tissue paper of claim 3, wherein said paper fibre comprises the mixture of broad-leaved wood fiber and needle-leaved wood fibre, and said broad-leaved wood fiber is at least 50% of said paper fibre, and said needle fiber is at least 10% of said paper fibre.

6. the tissue paper of claim 5, wherein said tissue paper comprises the layer of at least two stacks, internal layer and at least one skin that is connected with said internal layer.

7, the tissue paper of claim 6, wherein said tissue paper comprises the layer of three stacks, an internal layer and two skins, said internal layer is between said two skins.

8. the tissue paper of claim 7, wherein said internal layer comprise average length at least greater than 2.0 millimeters needle-leaved wood fibre, and said skin comprises average length less than 1.0 millimeters broad-leaved wood fiber.

9. the tissue paper of claim 8, wherein needle-leaved wood fibre comprises northern needlebush kraft fibers, and broad-leaved wood fiber comprises the eucalyptus kraft fibers.

10. the tissue paper of claim 9, wherein said particulate filler is a kaolin.

11. the tissue paper of claim 10, wherein said kaolin account for 8% to 20% of described tissue paper weight.

12. the tissue paper of claim 10, wherein said kaolin is made up of aluminium hydrosilicate, and it has the average quite sphere diameter greater than 0.5 micron.

13. the tissue paper of claim 12, wherein said kaolin have the average quite sphere diameter greater than 1.0 microns.

14. the tissue paper of claim 3, wherein said creped tissue paper is the page of pattern densification, causes high relatively tightness district to be distributed in the high bulk district.

15, the tissue paper of claim 14, wherein said high relatively tightness district is continuous, and the high bulk district is discontinuous.

16, the tissue paper of claim 15, wherein said particulate filler are kaolin.

17. the tissue paper of claim 16, wherein said kaolin account for 8% to 20% of described tissue paper weight.

18. the tissue paper of claim 16, wherein said kaolin is made up of aluminium hydrosilicate, and it has the average quite sphere diameter greater than 0.5 micron.

19. the tissue paper of claim 18, wherein said kaolin have the average quite sphere diameter greater than 1.0 microns.

20, the tissue paper of claim 3, wherein said particulate filler are kaolin.